CN102583336B - Preparation method of magnetic-functionalized graphene composite material - Google Patents
Preparation method of magnetic-functionalized graphene composite material Download PDFInfo
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- CN102583336B CN102583336B CN201210018658.6A CN201210018658A CN102583336B CN 102583336 B CN102583336 B CN 102583336B CN 201210018658 A CN201210018658 A CN 201210018658A CN 102583336 B CN102583336 B CN 102583336B
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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 of the magnetic-functionalized graphene composite material by solvent thermal reaction single stage method.
Background technology
Graphene is by the cellular lattice structure of the former molecular two-dimensional and periodic of monolayer carbon, 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 unique structure and excellent performance, as high theoretical surface is long-pending, high charge mobility, high Young's modulus, high thermal conductivity etc. caused the extensive concern of scientists.
Due to the potential application in fields such as material, chemistry, biomedicines, as 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 preparing magnetic-functionalized graphene composite material of report mainly contains two kinds both at home and abroad at present: one is single stage method, under solvent thermal conditioned disjunction alkaline condition, allow magnetic nano-particle presoma pyrolytic decomposition or precipitin reaction occurs, generate magnetic nanoparticle and also load on graphite oxide carrier.Chen YS (Chen YS, et al.J Mater.Chem 2009,19:2710-2714) etc. people has prepared the matrix material of graphene oxide load ferriferrous oxide nano-particle by chemical precipitation method, its method is that graphite oxide, iron(ic) chloride and iron protochloride are scattered in aqueous sodium hydroxide solution, then mixing solutions is stirred, be heated to 60 DEG C and keep 2h.Its solid support material is graphene oxide, belongs to isolator, poorly conductive; Ferriferrous oxide particles skewness, matrix material saturation magnetization is low.Another kind is two-step approach, first prepares magnetic nanoparticle, and recycling magnetic nanoparticle and the graphene oxide of crossing through surface modification carry out crosslinking reaction, obtain magnetic/functionalized graphene composite material.(the Zhang ZJ such as Zhang ZJ, et al.Nanoscale, 2011,3,1446-1450) prepare the graphene composite material of load ferriferrous oxide nano-particle by two-step approach, its method is first to utilize high-temperature decomposition reaction to prepare ferroferric oxide magnetic nano-particles, and carries out carboxylic acid, then carries out crosslinking reaction with the graphene oxide that Polystyrene is crossed.This preparation method can control the particle diameter of magnetic nanoparticle preferably, but preparation technology is loaded down with trivial details, is unfavorable for expanding production.
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 preparing has superparamagnetic characteristic and higher saturation magnetization, Graphene carrier conductivity is good, the ferroferric oxide nano granules of load is evenly distributed, particle is little, the preparation method of the magnetic-functionalized graphene composite material of better crystallinity degree.
Technical scheme of the present invention be by graphite oxide and acetyl acetone iron in quadrol/water mixed solvent, utilize the solvent thermal reaction of mixed solvent, directly one-step synthesis magnetic-functionalized graphene composite material.
The present invention includes following steps:
1) quadrol and water are made into mixed solvent, then by graphite oxide with acetyl acetone iron is ultrasonic is scattered in mixed solvent, obtain the quadrol/aqueous dispersions of graphite oxide and acetyl acetone iron;
2) by step 1) graphite oxide of gained and the quadrol/aqueous dispersions of acetyl acetone iron be transferred to the reaction kettle for reaction of inner liner polytetrafluoroethylene, obtains solid product;
3) by step 2) washing of the solid product of gained, then collect product with magnet, dry and obtain magnetic/functionalized graphene composite material.
In step 1) in, the volume ratio of described quadrol and water can be 9: 1; The mass ratio of described graphite oxide and acetyl acetone iron can be (1～9): 1; It is the ultrasonic processor of 90W that described ultrasonic dispersion can adopt power, and ultrasonic time can be 15h; The preparation method of described graphite oxide is as follows:
Take the commercially available Graphite Powder 99 of 2g and 1g SODIUMNITRATE in round-bottomed flask, slowly adding 46mL concentration is 98% sulfuric acid.Mixed solution stirs 15min under condition of ice bath, then adds several times 6g potassium permanganate, continues to stir after 30min, removes ice bath and continues and stir.After stirring 5h, first add 92mL deionized water, continue to stir 15min, then add 280mL deionized water in batches, add 10mL 30%H simultaneously
2o
2solution, continues to stir 30min, obtains yellow graphite oxide solution.After reaction finishes, mixture centrifugal 5min under 8000r/min condition is obtained to solid product.Adopt centrifugal method to wash and purifying solid product, it is dry that sample is placed in vacuum drying oven.
In step 2) in, the temperature of described reaction can be 200 DEG C, and the time of reaction can be 24h.
In step 3) in, described washing is water and washing with alcohol successively.
Beneficial effect of the present invention is as follows:
1) the present invention, taking the standby graphite oxide of Hummers legal system and commercially available acetyl acetone iron as raw material, prepares magnetic-functionalized graphene composite material by solvent thermal reaction, and the reduction of graphite oxide and the generation of ferroferric oxide nano granules complete simultaneously;
2) magnetic-functionalized graphene composite material that the present invention prepares, has superparamagnetic characteristic, and 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 graphene film carrier by changing the feed ratio of reactant;
4) preparation technology is simple, low to production unit requirement, is easy to suitability for industrialized production;
5) prepared magnetic-functionalized graphene composite material can be widely used in the field such as the electrode materials, pharmaceutical carrier, magnetic resonance radiography of energy storage device and the environmental pollutant separation of magnetic mediation.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of the embodiment of the present invention 1 prepared magnetic-functionalized graphene composite material.In Fig. 1, X-coordinate be diffraction angle 2 θ (°), ordinate zou is relative intensity; Curve a is G-Fe
3o
4, curve b is GFe
3o
4.
Fig. 2 is the energy spectrum analysis figure of the embodiment of the present invention 1 prepared magnetic-functionalized graphene composite material.In Fig. 2, X-coordinate is that ordinate zou is relative intensity in conjunction with energy (eV); Wherein, left peak is Fe (2p
3/2), right peak is Fe (2p
1/2).
Fig. 3 is the scanning electron microscope (SEM) photograph of the embodiment of the present 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 present 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 present 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 scanning electron microscope (SEM) photograph of the embodiment of the present 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 present invention 2 prepared magnetic-functionalized graphene composite materials.In Fig. 7, be labeled as 100nm.
Fig. 8 is the scanning electron microscope (SEM) photograph of the embodiment of the present 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 present 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 50mg graphite oxide and 50mg acetyl acetone iron is scattered in step 1) mixed solvent in, ultrasonic dispersion 15h; The mass ratio of described graphite oxide and acetyl acetone iron is 1: 1;
3) by step 2) mixing solutions of gained is transferred in the autoclave of inner liner polytetrafluoroethylene, at 200 DEG C, reacts 24h.
4) reaction is cooled to room temperature after finishing, and the product in polytetrafluoroethyllining lining is poured out.Gained solid water and ethanolic soln repeatedly wash, then collect product with magnet, and sample is dried and obtained magnetic/functionalized graphene composite material.
The magnetic-functionalized graphene composite material sample of gained in the present embodiment, through every sign, characterization result is referring to Fig. 1～5.
Diffraction peak by Fig. 1 (X-ray diffractogram of matrix material) shows, this matrix material is Graphene-Z 250.
Illustrated by Fig. 2 (EDAX results of matrix material), the nanoparticle of graphene film load is ferriferrous oxide particles.
Can be found out by Fig. 3 (scanning electron microscope (SEM) photograph of matrix material), ferriferrous oxide particles is attached on graphene film equably.
Can be found out by Fig. 4 (transmission electron microscope picture of matrix material), ferriferrous oxide particles is attached on graphene film equably, and Z 250 is the irregular particle that size is about 20～30nm.
Can be found out by Fig. 5 (the magnetic hysteresis loop figure of matrix material), magnetic hysteresis loop presents typical S type, and residual magnetization is tending towards 0, shows that matrix material has superparamagnetic characteristic.
Embodiment 2
1) preparation 50mL quadrol/water mixed solution (volume ratio is 9: 1).
2) take 70mg graphite oxide and 30mg acetyl acetone iron is scattered in step 1) mixed solvent in, ultrasonic dispersion 15h; The mass ratio of described graphite oxide and acetyl acetone iron is 7: 3.
3) by step 2) mixing solutions of gained is transferred in the autoclave of inner liner polytetrafluoroethylene, at 200 DEG C, reacts 24h.
4) reaction is cooled to room temperature after finishing, and the product in polytetrafluoroethyllining lining is poured out.Gained solid water and ethanolic soln repeatedly wash, then collect product with magnet, and sample is dried and obtained magnetic/functionalized graphene composite material.
The magnetic-functionalized graphene composite material sample obtaining in the present embodiment, its X-ray diffractogram and EDAX results are identical with embodiment 1, show that matrix material is is Graphene-Z 250, the nanoparticle of graphene film load is ferriferrous oxide particles.
Can be found out by Fig. 6 (scanning electron microscope (SEM) photograph of the matrix material that the present embodiment obtains), ferriferrous oxide particles is attached on graphene film equably.
Can be found out by Fig. 7 (transmission electron microscope picture of the matrix material that the present embodiment obtains), ferriferrous oxide particles is attached on graphene film equably, and Z 250 is the irregular particle that size is about 10～20nm.Compared with embodiment 1, the size of ferriferrous oxide particles is less, and the charge capacity on Graphene carrier is also less.
Embodiment 3
1) preparation 50mL quadrol/water mixed solution (volume ratio is 9: 1).
2) take 90mg graphite oxide and 10mg acetyl acetone iron is scattered in step 1) mixed solvent in, ultrasonic dispersion 15h; The mass ratio of described graphite oxide and acetyl acetone iron is 9: 1.
3) by step 2) mixing solutions of gained is transferred in the autoclave of inner liner polytetrafluoroethylene, at 200 DEG C, reacts 24h.
4) reaction is cooled to room temperature after finishing, and the product in polytetrafluoroethyllining lining is poured out.Gained solid water and ethanolic soln repeatedly wash, then collect product with magnet, and sample is dried and obtained magnetic/functionalized graphene composite material.
The magnetic-functionalized graphene composite material sample obtaining in the present embodiment, its X-ray diffractogram and EDAX results are identical with embodiment 2 with embodiment 1, show that matrix material is is Graphene-Z 250, the nanoparticle of graphene film load is ferriferrous oxide particles.
Can be found out by Fig. 8 (scanning electron microscope (SEM) photograph of the matrix material that the present embodiment obtains), ferriferrous oxide particles is sparsely attached on graphene film.
Can be found out by Fig. 9 (transmission electron microscope picture of the matrix material that the present embodiment obtains), ferriferrous oxide particles is sparsely attached on 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 less, and the charge capacity on Graphene carrier is also less.
Can be found out by above 3 embodiment, can control the size of ferriferrous oxide particles and the charge capacity on graphene film by changing the feed ratio of graphite oxide and acetyl acetone iron, graphite oxide and acetyl acetone weight of iron ratio are 1: 1 o'clock charge capacity maximum.
Claims (3)
1. a preparation method for magnetic-functionalized graphene composite material, is characterized in that comprising the following steps:
1) quadrol and water are made into mixed solvent, then by graphite oxide with acetyl acetone iron is ultrasonic is scattered in mixed solvent, obtain the quadrol/aqueous dispersions of graphite oxide and acetyl acetone iron; The volume ratio of described quadrol and water is 9: 1; The mass ratio of described graphite oxide and acetyl acetone iron is 1～9: 1;
The preparation method of described graphite oxide is as follows:
Take the commercially available Graphite Powder 99 of 2g and 1g SODIUMNITRATE in round-bottomed flask, slowly adding 46mL concentration is 98% sulfuric acid; Mixed solution stirs 15min under condition of ice bath, then adds several times 6g potassium permanganate, continues to stir after 30min, removes ice bath and continues and stir; After stirring 5h, first add 92mL deionized water, continue to stir 15min, then add 280mL deionized water in batches, add 10mL30%H simultaneously
2o
2solution, continues to stir 30min, obtains yellow graphite oxide solution; After reaction finishes, mixture centrifugal 5min under 8000r/min condition is obtained to solid product; Adopt centrifugal method to wash and purifying solid product, it is dry that sample is placed in vacuum drying oven;
2) by step 1) graphite oxide of gained and the quadrol/aqueous dispersions of acetyl acetone iron be transferred to the reaction kettle for reaction of inner liner polytetrafluoroethylene, obtains solid product; The temperature of described reaction is 200 DEG C, and the time of reaction is 24h;
3) by step 2) washing of the solid product of gained, then collect product with magnet, dry and obtain 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) in, described ultrasonic dispersion adopts the ultrasonic processor that power is 90W, and ultrasonic time is 15h.
3. the preparation method of a kind of magnetic-functionalized graphene composite material as claimed in claim 1, is characterized in that in step 3) in, described washing is water and washing with alcohol successively.
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| US10335775B2 (en) * | 2015-05-26 | 2019-07-02 | Council Of Scientific & Industrial Research | Magnetically separable iron-based heterogeneous catalysts for dehydrogenation of alcohols and amines |
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| CN103846076B (en) * | 2012-12-05 | 2015-12-23 | 河海大学 | A kind of preparation method of magnetic oxygenated Graphene |
| CN103127910B (en) * | 2013-03-07 | 2015-10-28 | 吴敏 | A kind of magnetic graphene, preparation method and its usage |
| CN103183343A (en) * | 2013-04-17 | 2013-07-03 | 桂林理工大学 | Preparation method of aminated magnetic graphene |
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| CN104909348B (en) * | 2015-05-12 | 2017-05-03 | 浙江理工大学 | Method for preparing oxidized graphene with high dispersibility based on microwave pretreatment |
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| KR102049574B1 (en) | 2015-10-30 | 2019-11-27 | 주식회사 엘지화학 | Method for preparation of magnetic iron oxide-graphene complex |
| CN108022706B (en) * | 2017-12-22 | 2020-01-07 | 湖南工程学院 | Preparation method of magnetic functionalized graphene composite material |
| CN108212127B (en) * | 2018-01-18 | 2020-02-18 | 河海大学 | Preparation method and application of functional nano composite hydrogel |
| CN109273285A (en) * | 2018-10-15 | 2019-01-25 | 河北工业大学 | A kind of preparation method of nickel-zinc ferrite/graphene composite material |
| CN113443618A (en) * | 2021-07-30 | 2021-09-28 | 江苏斯迪克新材料科技股份有限公司 | Magnetic graphene and preparation method thereof |
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| WO2009158117A2 (en) * | 2008-05-30 | 2009-12-30 | The Regents Of The University Of California | Chemical modulation of electronic and magnetic properties of graphene |
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