CN102583336A - Preparation method of magnetic-functionalized graphene composite material - Google Patents
Preparation method of magnetic-functionalized graphene composite material Download PDFInfo
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- CN102583336A CN102583336A CN2012100186586A CN201210018658A CN102583336A CN 102583336 A CN102583336 A CN 102583336A CN 2012100186586 A CN2012100186586 A CN 2012100186586A CN 201210018658 A CN201210018658 A CN 201210018658A CN 102583336 A CN102583336 A CN 102583336A
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Abstract
The invention provides a preparation method of a magnetic-functionalized graphene composite material, and relates to preparation of a graphene composite material. According to the invention, the preparation method is simple, the raw material is easily obtained, and the industrial production is easy; the prepared magnetic-functionalized graphene composite material has superparamagnetic property and is higher in saturated magnetization; and the graphene carrier is good in conductivity, and loaded ferroferric oxide nano particles are uniformly distributed, are small and are good in crystallizability. The preparation method comprises the following steps of: matching ethanediamine and water into a mixed solvent, then ultrasonically dispersing graphite oxide and iron acetylacetonate in the mixed solvent, and obtaining ethanediamine/dispersion of the graphite oxide and the iron acetylacetonate; transferring the ethanediamine/dispersion of the graphite oxide and the iron acetylacetonate into a reactor lined with polytetrafluoroethylene for reaction and obtaining solid products; and cleaning the solid products, collecting the products with a magnet, drying and obtaining the magnetic-functionalized graphene composite material.
Description
Technical field
The present invention relates to a kind of preparation of graphene composite material, especially relate to a kind of preparation method who passes through the magnetic/functionalized graphene composite material of solvent thermal reaction single stage method.
Background technology
The cellular lattice structure of two-dimensional and periodic that Graphene is made up of the monolayer carbon atom is up to now the thinnest two-dimensional nano material.From reported first such as Andre Geim in 2004 and Kostya Novoselov since its micromechanics strip preparation method; Graphene is just with its particular structure and excellent performance, and, high charge mobility long-pending like high theoretical surface, high Young's modulus, high thermal conductivity etc. have caused the extensive concern of scientists.
Because in the potential application in fields such as material, chemistry, biomedicine, like the target drug-carrying body of magnetic steering, nuclear magnetic resonance, electrode materials etc., the preparation of magnetic/functionalized graphene composite material and performance study are just receiving increasing concern.The method of the magnetic/functionalized graphene composite material of preparation of report mainly contains two kinds both at home and abroad at present: a kind of is single stage method; Under solvent thermal conditioned disjunction alkaline condition; Let magnetic nano-particle presoma pyrolytic decomposition or precipitin reaction takes place, generate magnetic nanoparticle and also load on the graphite oxide carrier.Chen YS (Chen YS; Et al.J Mater.Chem 2009; 19:2710-2714) wait the people to prepare the matrix material of graphene oxide load ferriferrous oxide nano-particle through chemical precipitation method; Its method is that graphite oxide, iron(ic)chloride and iron protochloride are scattered in the aqueous sodium hydroxide solution, then mixing solutions is stirred, and is heated to 60 ℃ and keep 2h.Its solid support material is a graphene oxide, belongs to isolator, poorly conductive; The ferriferrous oxide particles skewness, the matrix material saturation magnetization is low.Another kind is a two-step approach, at first prepares magnetic nanoparticle, utilizes magnetic nanoparticle again and carries out crosslinking reaction through the graphene oxide that surface-treated is crossed, and obtains magnetic/functionalized graphene composite material.(Zhang ZJ such as Zhang ZJ; Et al.Nanoscale, 2011,3; 1446-1450) prepare the graphene composite material that obtains the load ferriferrous oxide nano-particle through two-step approach; Its method is at first to utilize high-temperature decomposition reaction to prepare ferroferric oxide magnetic nano-particles, and carry out carboxylic acidization, and the graphene oxide with the PS modification carries out crosslinking reaction again.This preparation method can control the particle diameter of magnetic nanoparticle preferably, but preparation technology is loaded down with trivial details, is unfavorable for enlarging producing.
Summary of the invention
The object of the present invention is to provide that a kind of method is simple, raw material is easy to get, is easy to suitability for industrialized production; The magnetic/functionalized graphene composite material for preparing has ultra paramagnetic characteristic and higher saturation magnetization; The Graphene carrier conductivity is good; The ferroferric oxide nano granules of load is evenly distributed, and particle is little, the preparation method of the magnetic/functionalized graphene composite material of better crystallinity degree.
Technical scheme of the present invention be through graphite oxide and acetyl acetone iron in quadrol/water mixed solvent, utilize the solvent thermal reaction of mixed solvent, directly the magnetic/functionalized graphene composite material of one-step synthesis.
The present invention includes following steps:
1) quadrol and water are made into mixed solvent, again with graphite oxide and acetyl acetone iron ultra-sonic dispersion in mixed solvent, obtain the quadrol/aqueous dispersions of graphite oxide and acetyl acetone iron;
2) quadrol/aqueous dispersions of the graphite oxide of step 1) gained and acetyl acetone iron is transferred to the reaction kettle for reaction of inner liner polytetrafluoroethylene, solid product;
3) with step 2) washing of the solid product of gained, collect product with magnet again, oven dry obtains magnetic/functionalized graphene composite material.
In step 1), the volume ratio of said quadrol and water can be 9: 1; The mass ratio of said graphite oxide and acetyl acetone iron can be (1~9): 1; It is the ultrasonic processor of 90W that said ultra-sonic dispersion can adopt power, and ultrasonic time can be 15h; The preparation method of said graphite oxide is following:
Take by weighing commercially available Graphite Powder 99 of 2g and 1g SODIUMNITRATE in round-bottomed flask, slowly add 46mL concentration and be 98% sulfuric acid.Mixed solution stirs 15min under condition of ice bath, add 6g potassium permanganate more several times, after continuing to stir 30min, removes ice bath and continues and stir.Add the 92mL deionized water earlier after stirring 5h, continue to stir 15min, add the 280mL deionized water more in batches, add 10mL 30%H simultaneously
2O
2Solution continues to stir 30min, obtains xanchromatic graphite oxide solution.After reaction finished, centrifugal 5min under the 8000r/min condition got solid product with mixture.Adopt centrifugal method that solid product is washed and purifying, sample places vacuum drying oven dry.
In step 2) in, the temperature of said reaction can be 200 ℃, and the time of reaction can be 24h.
In step 3), said washing is water and washing with alcohol successively.
Beneficial effect of the present invention is following:
1) the present invention is a raw material with the graphite oxide and the commercially available acetyl acetone iron of the preparation of Hummers method, prepares magnetic/functionalized graphene composite material through solvent thermal reaction, and the reduction of graphite oxide and the generation of ferroferric oxide nano granules are accomplished simultaneously;
2) the magnetic/functionalized graphene composite material for preparing of the present invention has ultra paramagnetic characteristic, and the Graphene carrier conductivity is good, and the ferroferric oxide nano granules of load is evenly distributed, and particle is little, better crystallinity degree;
3) can control the size of ferroferric oxide nano granules and the charge capacity on the graphene film carrier through the feed ratio that changes reactant;
4) preparation technology is simple, and is low to the production unit requirement, is easy to suitability for industrialized production;
5) prepared magnetic/functionalized graphene composite material can be widely used in the fields such as environmental pollutant separation of electrode materials, pharmaceutical carrier, magnetic resonance radiography and the magnetic mediation of energy storage device.
Description of drawings
Fig. 1 is the X-ray diffractogram of the embodiment of the invention 1 prepared magnetic/functionalized graphene composite material.In Fig. 1, X-coordinate be diffraction angle 2 θ (°), ordinate zou is a relative intensity; Curve a is G-Fe
3O
4, curve b is GFe
3O
4
Fig. 2 is the ability spectrum analysis figure of the embodiment of the invention 1 prepared magnetic/functionalized graphene composite material.In Fig. 2, X-coordinate is bound energy (eV), and ordinate zou is a relative intensity; Wherein, left peak is Fe (2p
3/2), right peak is Fe (2p
1/2).
Fig. 3 is the sem photograph of the embodiment of the invention 1 prepared magnetic/functionalized graphene composite material.In Fig. 3, scale is 200 μ m.
Fig. 4 is the transmission electron microscope picture of the embodiment of the invention 1 prepared magnetic/functionalized graphene composite material.In Fig. 4, scale is 100nm.
Fig. 5 is the magnetic hysteresis loop figure of the embodiment of the invention 1 prepared magnetic/functionalized graphene composite material.In Fig. 5, X-coordinate is magneticstrength (Oe), and ordinate zou is the specific magnetising moment (emu/g).
Fig. 6 is the sem photograph of the embodiment of the invention 2 prepared magnetic/functionalized graphene composite materials.In Fig. 6, be labeled as 200nm.
Fig. 7 is the transmission electron microscope picture of the embodiment of the invention 2 prepared magnetic/functionalized graphene composite materials.In Fig. 7, be labeled as 100nm.
Fig. 8 is the sem photograph of the embodiment of the invention 3 prepared magnetic/functionalized graphene composite materials.In Fig. 8, be labeled as 400nm.
Fig. 9 is the transmission electron microscope picture of the embodiment of the invention 3 prepared magnetic/functionalized graphene composite materials.In Fig. 9, be labeled as 100nm.
Embodiment
Embodiment 1
1) preparation 50mL quadrol/water mixed solvent (volume ratio is 9: 1).
2) take by weighing the 50mg graphite oxide and 50mg acetyl acetone iron is scattered in the mixed solvent of step 1), ultra-sonic dispersion 15h; The mass ratio of said graphite oxide and acetyl acetone iron is 1: 1;
3) with step 2) mixing solutions of gained is transferred in the autoclave of inner liner polytetrafluoroethylene, at 200 ℃ of reaction 24h down.
4) reaction finishes postcooling to room temperature, and the product in the polytetrafluoroethyllining lining is poured out.Gained solid water and ethanolic soln repeatedly wash, and collect product with magnet again, and the sample oven dry obtains magnetic/functionalized graphene composite material.
The magnetic/functionalized graphene composite material sample of gained in the present embodiment characterizes through each item, and characterization result is referring to Fig. 1~5.
Diffraction peak by Fig. 1 (X-ray diffractogram of matrix material) shows that this matrix material is Graphene-Z 250.
Explain that by Fig. 2 (EDAX results of matrix material) nanoparticle of graphene film load is a ferriferrous oxide particles.
Can find out that by Fig. 3 (sem photograph of matrix material) ferriferrous oxide particles is equably attached on the graphene film.
Can be found out that by Fig. 4 (transmission electron microscope picture of matrix material) ferriferrous oxide particles is equably attached on the graphene film, Z 250 is the irregular particle that size is about 20~30nm.
Can find out that by Fig. 5 (the magnetic hysteresis loop figure of matrix material) magnetic hysteresis loop presents typical S type, residual magnetization is tending towards 0, shows that matrix material has ultra paramagnetic characteristic.
Embodiment 2
1) preparation 50mL quadrol/water mixed solution (volume ratio is 9: 1).
2) take by weighing the 70mg graphite oxide and 30mg acetyl acetone iron is scattered in the mixed solvent of step 1), ultra-sonic dispersion 15h; The mass ratio of said graphite oxide and acetyl acetone iron is 7: 3.
3) with step 2) mixing solutions of gained is transferred in the autoclave of inner liner polytetrafluoroethylene, at 200 ℃ of reaction 24h down.
4) reaction finishes postcooling to room temperature, and the product in the polytetrafluoroethyllining lining is poured out.Gained solid water and ethanolic soln repeatedly wash, and collect product with magnet again, and the sample oven dry obtains magnetic/functionalized graphene composite material.
Resulting magnetic/functionalized graphene composite material sample in the present embodiment; Its X-ray diffractogram is identical with embodiment 1 with EDAX results; Show that matrix material is to be Graphene-Z 250, the nanoparticle of graphene film load is a ferriferrous oxide particles.
Can find out that by Fig. 6 (sem photograph of the resulting matrix material of present embodiment) ferriferrous oxide particles is equably attached on the graphene film.
Can be found out that by Fig. 7 (transmission electron microscope picture of the resulting matrix material of present embodiment) ferriferrous oxide particles is equably attached on the graphene film, Z 250 is the irregular particle that size is about 10~20nm.Compare with embodiment 1, the size of ferriferrous oxide particles is littler, and the charge capacity on the Graphene carrier is also littler.
Embodiment 3
1) preparation 50mL quadrol/water mixed solution (volume ratio is 9: 1).
2) take by weighing the 90mg graphite oxide and 10mg acetyl acetone iron is scattered in the mixed solvent of step 1), ultra-sonic dispersion 15h; The mass ratio of said graphite oxide and acetyl acetone iron is 9: 1.
3) with step 2) mixing solutions of gained is transferred in the autoclave of inner liner polytetrafluoroethylene, at 200 ℃ of reaction 24h down.
4) reaction finishes postcooling to room temperature, and the product in the polytetrafluoroethyllining lining is poured out.Gained solid water and ethanolic soln repeatedly wash, and collect product with magnet again, and the sample oven dry obtains magnetic/functionalized graphene composite material.
Resulting magnetic/functionalized graphene composite material sample in the present embodiment; Its X-ray diffractogram is identical with embodiment 2 with embodiment 1 with EDAX results; Show that matrix material is to be Graphene-Z 250, the nanoparticle of graphene film load is a ferriferrous oxide particles.
Can find out that by Fig. 8 (sem photograph of the resulting matrix material of present embodiment) ferriferrous oxide particles is sparsely attached on the graphene film.
Can find out by Fig. 9 (transmission electron microscope picture of the resulting matrix material of present embodiment); Ferriferrous oxide particles is sparsely attached on the graphene film; Z 250 is the irregular particle that size is about 10~20nm; Compare with embodiment 2 with embodiment 1, the size of ferriferrous oxide particles is littler, and the charge capacity on the Graphene carrier is also littler.
Can find out by above 3 embodiment; Can control the size of ferriferrous oxide particles and the charge capacity on graphene film through the feed ratio that changes graphite oxide and acetyl acetone iron, graphite oxide and acetyl acetone weight of iron ratio are that 1: 1 o'clock charge capacity is maximum.
Claims (7)
1. the preparation method of a magnetic/functionalized graphene composite material is characterized in that may further comprise the steps:
1) quadrol and water are made into mixed solvent, again with graphite oxide and acetyl acetone iron ultra-sonic dispersion in mixed solvent, obtain the quadrol/aqueous dispersions of graphite oxide and acetyl acetone iron;
2) quadrol/aqueous dispersions of the graphite oxide of step 1) gained and acetyl acetone iron is transferred to the reaction kettle for reaction of inner liner polytetrafluoroethylene, solid product;
3) with step 2) washing of the solid product of gained, collect product with magnet again, oven dry obtains magnetic/functionalized graphene composite material.
2. the preparation method of a kind of magnetic/functionalized graphene composite material as claimed in claim 1 is characterized in that in step 1), and the volume ratio of said quadrol and water is 9: 1.
3. the preparation method of a kind of magnetic/functionalized graphene composite material as claimed in claim 1 is characterized in that in step 1), and the mass ratio of said graphite oxide and acetyl acetone iron is 1~9: 1.
4. the preparation method of a kind of magnetic/functionalized graphene composite material as claimed in claim 1 is characterized in that in step 1), and it is the ultrasonic processor of 90W that said ultra-sonic dispersion adopts power, and ultrasonic time is 15h.
5. the preparation method of a kind of magnetic/functionalized graphene composite material as claimed in claim 1 is characterized in that in step 1), and the preparation method of said graphite oxide is following:
Take by weighing commercially available Graphite Powder 99 of 2g and 1g SODIUMNITRATE in round-bottomed flask, slowly add 46mL concentration and be 98% sulfuric acid; Mixed solution stirs 15min under condition of ice bath, add 6g potassium permanganate more several times, after continuing to stir 30min, removes ice bath and continues and stir; Add the 92mL deionized water earlier after stirring 5h, continue to stir 15min, add the 280mL deionized water more in batches, add 10mL 30%H simultaneously
2O
2Solution continues to stir 30min, obtains xanchromatic graphite oxide solution; After reaction finished, centrifugal 5min under the 8000r/min condition got solid product with mixture; Adopt centrifugal method that solid product is washed and purifying, sample places vacuum drying oven dry.
6. the preparation method of a kind of magnetic/functionalized graphene composite material as claimed in claim 1 is characterized in that in step 2) in, the temperature of said reaction is 200 ℃, the time of reaction is 24h.
7. the preparation method of a kind of magnetic/functionalized graphene composite material as claimed in claim 1 is characterized in that in step 3), and said washing is water and washing with alcohol successively.
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CN103127910A (en) * | 2013-03-07 | 2013-06-05 | 吴敏 | Magnetic graphene as well as preparation method and application thereof |
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