CN103373725B - Preparation method of crystalloid graphite micropowder with unidirectional electromagnetic property - Google Patents
Preparation method of crystalloid graphite micropowder with unidirectional electromagnetic property Download PDFInfo
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- CN103373725B CN103373725B CN201210128546.6A CN201210128546A CN103373725B CN 103373725 B CN103373725 B CN 103373725B CN 201210128546 A CN201210128546 A CN 201210128546A CN 103373725 B CN103373725 B CN 103373725B
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Abstract
The invention discloses a preparation method of crystalloid graphite micropowder with unidirectional electromagnetic property. The preparation method comprises the following steps of: firstly uniformly mixing a graphite solution and an Fe<2+>/Fe<3+> mixed solution; then pouring a mixed solution into a three-grade flask inside a constant temperature water bath; then adding Na2CO3 liquid to the mixed solution till the reacted solution is alkaline and PH=7.8-9; then removing the reacted solution to an other higher constant temperature water bath to crystallize for 4-5 hours; finally washing, and drying the sample to obtain the magnetic graphite micropowder with magnetic nano particles attached. The method disclosed by the invention is simple in process, low in production cost and suitable for industrialized production; the prepared magnetic graphite micropowder has the advantages of good electricity conductive property and magnetic conductive property, is an excellent raw material of an electromagnetic shielding material and has a good application prospect in the fields of electron, electrics, communication, aviation, military and the like.
Description
Technical field
The invention belongs to Preparation Technique of Powders field, is more particularly a kind of for electromagnetic shielding, the graphite composite powder preparation method with conductive magneto-conductive.
Background technology
Electromagnetic shielding is the important means of electromagnetism interference, traditional electromagnetic shielding material is top layer conductivity type shielding material and filled composite type shielding material mainly, and top layer conductive shielding material the conductive filler material such as metal-powder, carbon black and macromolecular material is mixed with to form or make insulating material surface obtain very thin conductive metal layer by physico-chemical process and reach the effect of shielding.Filled composite shielding material is the electromagnetic shielding material processed through injection or extrusion moulding by macromolecule matrix and conductive filler material.Although these traditional shielding materials can reach the effect of shielding, shielding properties is general, and the frequency band range of shielding is very narrow, thus limits the application of these shielding materials.Theoretical according to electromagnetic shielding, the electromagnetic shielding material of excellent property should have higher electric conductivity and permeability.And Novel shielding material is while emphasizing shielding bandwidth sum high shielding properties, and the shielding material that development quality is light is the emphasis of this area research now.
Graphite is that a kind of excellent conductive filler material, the particularly graphite expanded graphite obtained by after intercalation has high specific conductivity and large surface-area, thus imparts the good electromagnetism of expanded graphite and cover performance.Expanded graphite is had good effectiveness by the graphite gasket that high pressure is suppressed by D.D.L.Chng, and this material also has excellent thermostability, chemical stability and low thermal expansivity, but the shielding material manufactured thus is diamagnetic.Thus, the shielding frequency range of this material is very limited.In order to improve the deficiency of graphite-based shielding material in this, a lot of research worker considers in graphite, to add magnetic substance to improve the shielding properties of graphite-based shielding material.
Summary of the invention
Object of the present invention provides a kind of preparation method with the Scaly graphite micro mist of unidirectional electrical magnetic properties, and the graphite-based shielding material that the graphite microparticles made with utilizing the inventive method is made has better shielding properties and comparatively ideal shielding frequency range.
Technical scheme of the present invention is such: a kind of preparation method with the Scaly graphite micro mist of unidirectional electrical magnetic properties, realizes as follows:
One, take a certain amount of graphite dispersion in liquid medium, form graphite dispersing solution, wherein, the weight ratio of graphite and liquid medium is 1: 10-70
Two, take divalent iron salt, trivalent iron salt at 2.0: 1-5.5: 1 in molar ratio, be mixed with the iron ion mixing solutions that concentration is 0.2-0.8M;
Three, after above-mentioned graphite dispersing solution being mixed with the ratio that volume ratio is 1: 1-6: 1 with iron ion mixing solutions, be placed in 35 DEG C of waters bath with thermostatic control, and stir and make it mix in 15 minutes;
Four, in the mixing solutions of step 3 gained, the Na that concentration is 0.55M is added
2cO
3liquid also ceaselessly stirs, until solution alkaline;
Five, the solution of step 4 gained to be moved in 65 DEG C of waters bath with thermostatic control crystallization 3.5 hours;
Six, the solution after washing crystallization, until washings is in neutral, finally adopt magnetic separation technique to isolate throw out in solution, namely oven dry, pulverizing obtain and are attached with magnetic Fe
3o
4the powdered graphite of nanoparticle.
Liquid medium in above-mentioned steps one is the organic or inorganic solution of soluble graphite.
In above-mentioned steps two, divalent iron salt and trivalent iron salt are the molysite not containing strong oxidizing property acid group.
Above-mentioned divalent iron salt is FeCl
2or FeSO
4.
Above-mentioned trivalent iron salt is FeCl
3or Fe
2(SO4)
3.
In above-mentioned steps three, reaction is carried out under water bath with thermostatic control.
In above-mentioned steps four, the alkali lye added in mixing solutions is middle aqueous alkali.
After adopting such scheme, graphite microparticles prepared by the present invention has the characteristic of conduction, magnetic conduction concurrently, compensate for conventional graphite and only has electroconductibility and do not have magnetic deficiency; And preparation technology of the present invention simple, be easy to industrialization and produce.Prepare electromagnetic shielding material with graphite microparticles prepared by the present invention and there is the features such as density is low, lightweight, the inner shield of ultra-wideband scope is effective, can be applicable to the broadband electromagnetical shielding material in electromagnetic interference, electromagnetic pollution, communication and areas of information technology, at electronics, electrically, communication, aviation and military field have good application prospect.
Embodiment
A kind of preparation method with the Scaly graphite micro mist of unidirectional electrical magnetic properties of the present invention, realizes by following several embodiment:
Embodiment 1:
1) the graphite alcohol dispersion liquid that 0.5000g2000 order graphite is mixed with 50ml is taken; Take 0.8341gFeSO
4, 6H
2o, 0.1622gFeCl
3.7H
2o is mixed with the mixing solutions of 50ml molysite.
2) above-mentioned two kinds of solution are poured in uncovered there-necked flask, are placed in 30 DEG C of water-baths, and stir 15 minutes with agitator, make it mix.
3) to step 2) the mixed solution and dripping concentration of gained is the Na of 0.4mol/l
2cO
3solution, drips Na
2cO
3while ceaselessly stirred solution, until the PH=8.9 of solution.
4) by step 3) solution of gained to be transferred in 50 DEG C of water-baths crystallization 2 hours, then by the throw out distilled water wash that obtains after crystallization repeatedly, until the PH=7.0 of washings.
5) adopt magnetic separation technique to be separated by throw out, dried by isolated throw out with vacuum drying oven, pulverizing just obtains and is attached with Fe
3o
42000 order graphite microparticles of magnetic nano-particle.
Embodiment 2:
1) take the graphite alcohol dispersion liquid that 0.5000g3000 order graphite is mixed with 50ml, take 0.8341gFeSO
4.6H
2o, 0.1622gFeCl
3.7H
2o is mixed with the mixing solutions of 50ml molysite.
2) above-mentioned two kinds of solution are poured in uncovered there-necked flask, are placed in 30 DEG C of water-baths, and stir 15 minutes with agitator, make it mix.
3) to step 2) drip the Na that concentration is 0.5mol1/l in the towering conjunction solution of gained
2cO
3solution, drips Na
2cO
3ceaselessly stirred solution while solution, until the PH=8.9 of solution.
4) by step 3) solution of gained to be transferred in 35 DEG C of water-baths crystallization 2 hours, then by the throw out distilled water wash that obtains after crystallization repeatedly, until the PH=7.0 of washings.
5) adopt magnetic separation technique to be separated by throw out, dried by isolated throw out with vacuum drying oven, pulverizing just obtains and is attached with Fe
3o
4the order graphite microparticles of magnetic nano-particle.
Claims (6)
1. there is a preparation method for the Scaly graphite micro mist of unidirectional electrical magnetic properties, it is characterized in that: realize as follows:
1) take a certain amount of graphite dispersion in alcohol, form graphite alcohol dispersion liquid, wherein, the weight ratio of graphite and alcohol is 1: 10-70;
2) take divalent iron salt, trivalent iron salt at 2.0: 1-5.5: 1 in molar ratio, be mixed with the iron ion mixing solutions that concentration is 0.2-0.8M;
3) after above-mentioned graphite dispersing solution being mixed with the ratio that volume ratio is 1: 1-6: 1 with iron ion mixing solutions, be placed in 35 DEG C of waters bath with thermostatic control, and stir and make it mix in 15 minutes;
4) to step 3) add the Na2CO3 liquid that concentration is 0.55 in the mixing solutions of gained, and ceaselessly stir, until solution ph is 7.5-8.9;
5) by step 4) solution of gained to move in 65 DEG C of waters bath with thermostatic control crystallization 3.5 hours;
6) solution after washing crystallization, until washings is in neutral, finally adopt magnetic separation technique to isolate throw out in solution, namely oven dry, pulverizing obtain the graphite microparticles being attached with magnetic Fe_3O_4 nanoparticle.
2. the preparation method with the Scaly graphite micro mist of unidirectional electrical magnetic properties according to claim 1, is characterized in that: in above-mentioned steps two, and divalent iron salt and trivalent iron salt are the molysite not containing strong oxidizing property acid group.
3. the preparation method with the Scaly graphite micro mist of unidirectional electrical magnetic properties according to claim 2, is characterized in that: above-mentioned divalent iron salt is FeCl2 or FeSO4.
4. the preparation method with the Scaly graphite micro mist of unidirectional electrical magnetic properties according to claim 2, is characterized in that: above-mentioned trivalent iron salt is FeCl3 or Fe2 (SO4) 3.
5. the preparation method with the powdered graphite of electromagnetic property according to claim 1, above-mentioned steps 3) in, reaction is carried out under water bath with thermostatic control.
6. the preparation method with the powdered graphite of electromagnetic property according to claim 1, is characterized in that: above-mentioned steps 4) in, the alkali lye added in mixing solutions is middle aqueous alkali.
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|---|---|---|---|
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| CN201210128546.6A CN103373725B (en) | 2012-04-28 | 2012-04-28 | Preparation method of crystalloid graphite micropowder with unidirectional electromagnetic property |
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| CN103373725B true CN103373725B (en) | 2015-07-15 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837971A (en) * | 2010-05-14 | 2010-09-22 | 东华大学 | Method for preparing graphene/Fe3O4 composite powder by alcohol thermal method |
| CN101941842A (en) * | 2010-10-11 | 2011-01-12 | 东华大学 | Method for preparing graphene loaded ferroferric oxide magnetic nanometer particle composite material |
| CN102173411A (en) * | 2011-01-13 | 2011-09-07 | 东华大学 | Preparation method of water-dispersible graphene/ferroferric oxide (Fe3O4) composite powder |
| KR20110119164A (en) * | 2010-04-26 | 2011-11-02 | 포항공과대학교 산학협력단 | Hybrid material comprising grapheme and iron oxide, method for manufacturing thereof and apparatus for treating waste water using thereof |
| CN102352215A (en) * | 2011-07-28 | 2012-02-15 | 西北工业大学 | Preparation method of electromagnetic double-complex nanometer microwave absorbent Fe3O4/NanoG |
-
2012
- 2012-04-28 CN CN201210128546.6A patent/CN103373725B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20110119164A (en) * | 2010-04-26 | 2011-11-02 | 포항공과대학교 산학협력단 | Hybrid material comprising grapheme and iron oxide, method for manufacturing thereof and apparatus for treating waste water using thereof |
| CN101837971A (en) * | 2010-05-14 | 2010-09-22 | 东华大学 | Method for preparing graphene/Fe3O4 composite powder by alcohol thermal method |
| CN101941842A (en) * | 2010-10-11 | 2011-01-12 | 东华大学 | Method for preparing graphene loaded ferroferric oxide magnetic nanometer particle composite material |
| CN102173411A (en) * | 2011-01-13 | 2011-09-07 | 东华大学 | Preparation method of water-dispersible graphene/ferroferric oxide (Fe3O4) composite powder |
| CN102352215A (en) * | 2011-07-28 | 2012-02-15 | 西北工业大学 | Preparation method of electromagnetic double-complex nanometer microwave absorbent Fe3O4/NanoG |
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Effective date of registration: 20160525 Address after: 321200 Zhejiang province Wuyi County Hushan Street No. 44 Patentee after: Xia Lihong Address before: 321200 Zhejiang province Wuyi County Hushan Street No. 44 Patentee before: Xia Huasong |
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