CN1773638A - Method for producing magnetic powder by form method - Google Patents
Method for producing magnetic powder by form method Download PDFInfo
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- CN1773638A CN1773638A CN 200510086823 CN200510086823A CN1773638A CN 1773638 A CN1773638 A CN 1773638A CN 200510086823 CN200510086823 CN 200510086823 CN 200510086823 A CN200510086823 A CN 200510086823A CN 1773638 A CN1773638 A CN 1773638A
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Abstract
A method for preparing magnetic power by template includes preparing polystyrene microbial by emulsion polymerization and carrying out surface modification on it to change its hydrophilic surface to be oleophylic surface as well as using it as growing template of magnetic power, dispersing said template in metal salt solution and adding NaOH or KOH for forming precipitation under strong agitation and in ultrasonic treatment, adding reducer when said unit is heated up to certain temperature to generate metal or its alloy on original position of template, obtaining magnetic power after washing and drying.
Description
Technical field:
The invention belongs to the Magnaglo preparing technical field, particularly relate to the method that a kind of template prepares Magnaglo, prepared Magnaglo is used as magnetic functional material, can be used for fields such as radar-wave absorbing, electromagnetic compatibility.This method can be used for the preparation of nucleocapsid structure organic/inorganic composite material.
Background technology:
In the development process of new material, composite material of core-shell structure is because the variation of its composition, size and arrangement architecture can bring various different physicochemical properties and extremely attention.People wish that two or more materials have the different materials characteristic concurrently or produce unique characteristics such as light, electricity, magnetic and catalysis by compound the reaching of microcosmic.Because the particularity of composite material of core-shell structure preparation, research at present mainly concentrate on the outer polymeric material field that coats of inorganic material (being mainly oxide), as TiO
2, SiO
2, CaCO
3Coat organic substances such as polystyrene Deng powder surface, Fe
3O
4, MnO
2Coat organic materials such as polypyrrole, polyaniline outward Deng oxide.And outside organic material, aspect the original position synthetic inorganic material, particularly use polystyrene (PSt) to rarely have relevant report as the synthetic metal dust aspect of template.Main at present research concentrates on sol-gal process, coprecipitation, is implemented in inorganic material surface and coats TiO
2, SiO
2Deng material.
In the development process of absorbing material, shielding material,, can realize by strengthening powder granularity for reaching good low frequency performance; Magnetic-particle live part the most then is its particle top layer, and the Magnaglo of employing nucleocapsid structure can significantly improve the utilance of material; Because the general density of soft magnetic metal powder is bigger, higher content of powder has not only increased device weight, and meanwhile material usage also significantly increases; Adopt template to prepare this class soft magnetic metal powder and can effectively control powder diameter, and effectively reduce powder density, be suitable for fields such as radar-wave absorbing and electromagnetic shielding.
Summary of the invention:
The object of the invention is to provide a kind of template to prepare the method for Magnaglo, has nucleocapsid structure, has magnetic and lighter weight.In addition, the density of powder can be regulated according to coating thickness, and outer clad material also can be done corresponding change as required.
Technical scheme of the present invention is: adopt emulsion polymerization to prepare polystyrene microsphere, and it is carried out surface modification, it is hydrophilic that microsphere surface is become by oleophylic, and with this template as the Magnaglo growth; Get above-mentioned template (polystyrene microsphere after the modification) and be distributed in the metal salt solution, in strong agitation or sonicated, add NaOH (or KOH) and form precipitation; After above-mentioned system is heated to uniform temperature, add suitable reducing agent, metal or its alloy original position on template generated, through cleaning, dry Magnaglo.
The concrete technology of the present invention is:
1. remove ionized water 50～200ml, styrene 1～10ml, lauryl sodium sulfate 0.005～0.05g, magnetic stirrer stirred after 0.5～2 hour, begin to be warming up to 60～90 ℃, and continue to stir, in 0.5～2 hour, dropwise add the persulfate aqueous solution of 1～10ml 0.1～5%.Keep temperature to continue to stir 2～6 hours.
2. in above-mentioned system, add 0.05～2ml coupling agent, in 0.5～2 hour, dropwise add the persulfate aqueous solution of 1～10ml0.1～5%.Finished to react through 3～8 hours again.
3. get the emulsion 1～5ml of step b preparation, be diluted to 30～100ml with deionized water, in stirring, add in 5～20g solubility cobalt salt, molysite, nickel salt or its mixture any one, dissolving back sonicated or strong agitation are 0.5～2 hour fully, add 5～20g NaOH or KOH gradually, process sonic oscillation or brute force are warming up to 60～90 ℃ after being stirred to evenly, add hydrazine hydrate or NaBH gradually
4Reducing agent 0.5～10g continues reaction 10～30 minutes; Through dry after cleaning, the magnetic separation, obtain having the Magnaglo of nucleocapsid structure.
The mixture of solubility cobalt salt of the present invention, molysite, nickel salt is 2～3 kinds mixing in cobalt salt, molysite, the nickel salt.
The invention has the advantages that: polystyrene moulding can change the ratio of monomer and surfactant as required to adjust particle size; Slaine can be the mixture of single slaine or several slaines as required; Coating thickness is determined by slaine content; Have the hydrophilic end oleophylic structure of an end after the used coupling agent hydrolysis, can extensively adopt coupling agents such as silane, titanate esters, preferentially recommend silane coupling agents such as KH550, KH560, KH570, A151; Used reducing agent can be hydrazine hydrate, polyalcohol, NaBH
4Deng reducing agent; Prepared Magnaglo granularity, controllable density can be used for radar-wave absorbing and electromagnetic shielding field.
Description of drawings:
Accompanying drawing that the present invention comprises is used to provide to further understanding of the present invention.
In the accompanying drawings:
Fig. 1: the Co powder microscopic appearance that does not adopt the template preparation;
Fig. 2: the PSt-Co microscopic appearance of template preparation;
Fig. 3: the X ray diffracting spectrum that does not adopt the Co powder of template preparation;
Fig. 4: the X ray diffracting spectrum of the PSt-Co powder of template preparation;
Embodiment:
By instantiation technical scheme of the present invention is further described.
Embodiment 1:
Get styrene 10ml, lauryl sodium sulfate 0.05g, deionized water 100ml, magnetic stirrer stir and continue after 1 hour to stir, and begin to be warming up to 75 ℃, dropwise add the persulfate aqueous solution of 5ml 1% in 1 hour.Keep temperature to continue to stir 3 hours.
Add 0.5ml silane coupler (KH570) in above-mentioned system, in 1 hour, dropwise add the persulfate aqueous solution of 5ml 1%.Finished to react through 6 hours again.
Prepared emulsion 1ml of second step is diluted to 50ml with deionized water, adds 10g CoCl in stirring
26H
2O, dissolving back sonicated is 30 minutes fully, adds 8g NaOH gradually, after sonic oscillation and powerful the stirring, is warming up to 80 ℃, adds hydrazine hydrate 5g (85%) gradually, continues reaction 20 minutes.Through dry after cleaning, the magnetic separation, get ultra-fine tool nucleocapsid structure PSt-Co powder.
Embodiment 2:
Get styrene 5ml, lauryl sodium sulfate 0.02g, deionized water 100ml, magnetic stirrer stir and continue after 1 hour to stir, and begin to be warming up to 70 ℃, dropwise add the persulfate aqueous solution of 3ml 1% in 1 hour.Keep temperature to continue to stir 4 hours.
Add 0.2ml silane coupler (KH570) in above-mentioned system, in 1 hour, dropwise add the persulfate aqueous solution of 3ml 1%.Finished to react through 5 hours again.
Prepared emulsion 3ml of second step is diluted to 50ml with deionized water, adds 8gNiCl in stirring
26H
2O, dissolving back sonicated is 1 hour fully, adds 6g NaOH gradually, after sonic oscillation and powerful the stirring, is warming up to 75 ℃, adds hydrazine hydrate 3g (85%) gradually, continues reaction 30 minutes.Through dry after cleaning, the magnetic separation, get ultra-fine tool nucleocapsid structure PSt-Ni powder.
Embodiment 3:
Get styrene 10ml, lauryl sodium sulfate 0.05g, deionized water 100ml, magnetic stirrer stir and continue after 1 hour to stir, and begin to be warming up to 75 ℃, dropwise add the persulfate aqueous solution of 5ml 1% in 1 hour.Keep temperature to continue to stir 3 hours.
Add 0.5ml silane coupler (A151) in above-mentioned system, in 1 hour, dropwise add the persulfate aqueous solution of 5ml 1%.Finished to react through 6 hours again.
Prepared emulsion 1ml of second step is diluted to 50ml with deionized water, adds 5gNiCl in stirring
26H
2O, 5gFeCl
36H
2O dissolved the back sonicated 1 hour fully, added 8g NaOH gradually, after sonic oscillation and powerful the stirring, was warming up to 75 ℃, added NaBH gradually
40.8g, continue reaction 20 minutes.Through dry after cleaning, the magnetic separation, get ultra-fine tool nucleocapsid structure PSt-Fe/Ni powder.
Embodiment 4:
Get styrene 10ml, lauryl sodium sulfate 0.05g, deionized water 100ml, magnetic stirrer stir and continue after 1 hour to stir, and begin to be warming up to 75 ℃, dropwise add the persulfate aqueous solution of 5ml 1% in 1 hour.Keep temperature to continue to stir 3 hours.
Add 0.5ml silane coupler (KH570) in above-mentioned system, in 1Hr, dropwise add the persulfate aqueous solution of 5ml 1%.Finished to react through 6 hours again.
Prepared emulsion 1ml of second step is diluted to 50ml with deionized water, adds 5gCoCl in stirring
26H
2O, 5gFeCl
36H
2O dissolved the back sonicated 1 hour fully, added 8g NaOH gradually, after sonic oscillation and powerful the stirring, was warming up to 75 ℃, added NaBH gradually
40.8g, continue reaction 20 minutes.Through dry after cleaning, the magnetic separation, get ultra-fine tool nucleocapsid structure PSt-Fe/Co powder.
Claims (2)
1, a kind of template prepares the method for Magnaglo, it is characterized in that: concrete technology is:
A. remove ionized water 50～200ml, styrene 1～10ml, lauryl sodium sulfate 0.005～0.05g, magnetic stirrer stirred after 0.5～2 hour, begin to be warming up to 60～90 ℃, and continue to stir, in 0.5～2 hour, dropwise add the persulfate aqueous solution of 1～10ml 0.1～5%, keep temperature to continue to stir 2～6 hours;
B. in the system of a step, add 0.05～2ml coupling agent, in 0.5～2 hour, dropwise add the persulfate aqueous solution of 1～10ml 0.1～5%, finished to react through 3～8 hours again;
C. get the emulsion 1～5ml of step b preparation, be diluted to 30～100ml with deionized water, in stirring, add in 5～20g solubility cobalt salt, molysite, nickel salt or its mixture any one, dissolving back sonicated or strong agitation are 0.5～2 hour fully, add 5～20g NaOH or KOH gradually, process sonic oscillation or brute force are warming up to 60～90 ℃ after being stirred to evenly, add hydrazine hydrate or NaBH gradually
4Reducing agent 0.5～10g continues reaction 10～30 minutes; Through dry after cleaning, the magnetic separation, obtain having the Magnaglo of nucleocapsid structure.
2, in accordance with the method for claim 1, it is characterized in that: the mixture of described solubility cobalt salt, molysite, nickel salt is 2～3 kinds mixing in cobalt salt, molysite, the nickel salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510086823 CN1773638B (en) | 2005-11-10 | 2005-11-10 | Method for producing magnetic powder by form method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510086823 CN1773638B (en) | 2005-11-10 | 2005-11-10 | Method for producing magnetic powder by form method |
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| Publication Number | Publication Date |
|---|---|
| CN1773638A true CN1773638A (en) | 2006-05-17 |
| CN1773638B CN1773638B (en) | 2010-04-21 |
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ID=36760534
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510086823 Expired - Fee Related CN1773638B (en) | 2005-11-10 | 2005-11-10 | Method for producing magnetic powder by form method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103374203A (en) * | 2012-04-24 | 2013-10-30 | 比亚迪股份有限公司 | Electromagnetic shielding material and preparation method of same |
| CN107029798A (en) * | 2017-04-12 | 2017-08-11 | 山西大学 | A kind of preparation method and application of hollow magnetic nanoparticle |
| CN108500292A (en) * | 2018-04-08 | 2018-09-07 | 合肥学院 | Preparation method of chain-like metallic nickel nano powder |
| CN112077332A (en) * | 2020-09-11 | 2020-12-15 | 广东工业大学 | Carbon-coated magnetic metal simple substance composite material and preparation method and application thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1293969C (en) * | 2003-11-14 | 2007-01-10 | 中国科学院化学研究所 | Method for preparing nano metal and bimetal hollow ball |
| CN1218974C (en) * | 2003-12-30 | 2005-09-14 | 上海交通大学 | Preparation method of high magnetism content magnetic polymer particle |
| CN100340299C (en) * | 2004-06-22 | 2007-10-03 | 北京倍爱康生物技术股份有限公司 | Method for preparing radioactive nuclide magnetic microsphere used in vivo |
-
2005
- 2005-11-10 CN CN 200510086823 patent/CN1773638B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103374203A (en) * | 2012-04-24 | 2013-10-30 | 比亚迪股份有限公司 | Electromagnetic shielding material and preparation method of same |
| CN107029798A (en) * | 2017-04-12 | 2017-08-11 | 山西大学 | A kind of preparation method and application of hollow magnetic nanoparticle |
| CN108500292A (en) * | 2018-04-08 | 2018-09-07 | 合肥学院 | Preparation method of chain-like metallic nickel nano powder |
| CN108500292B (en) * | 2018-04-08 | 2021-03-23 | 合肥学院 | Preparation method of chain-like metallic nickel nano powder |
| CN112077332A (en) * | 2020-09-11 | 2020-12-15 | 广东工业大学 | Carbon-coated magnetic metal simple substance composite material and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN1773638B (en) | 2010-04-21 |
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| C14 | Grant of patent or utility model | ||
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| CB03 | Change of inventor or designer information |
Inventor after: Gao Xuexu Inventor after: Zhou Zhibiao Inventor after: Mao Weimin Inventor after: Feng Huiping Inventor before: Guo Zhimeng Inventor before: Zhou Zhibiao Inventor before: Mao Weimin Inventor before: Feng Huiping |
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| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: GUO ZHIMENG ZHOU ZHIBIAO MAO WEIMIN FENG HUIPING TO: GAO XUEXU ZHOU ZHIBIAO MAO WEIMIN FENG HUIPING |
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Ningde Xingyu Technology Co., Ltd. Assignor: University of Science and Technology Beijing Contract record no.: 2010990000943 Denomination of invention: Method for producing magnetic powder by form method Granted publication date: 20100421 License type: Exclusive License Open date: 20060517 Record date: 20101203 |
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Granted publication date: 20100421 Termination date: 20121110 |