CN105251448B - A kind of preparation method of magnetic graphene composite - Google Patents
A kind of preparation method of magnetic graphene composite Download PDFInfo
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- CN105251448B CN105251448B CN201510805318.1A CN201510805318A CN105251448B CN 105251448 B CN105251448 B CN 105251448B CN 201510805318 A CN201510805318 A CN 201510805318A CN 105251448 B CN105251448 B CN 105251448B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 64
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000010521 absorption reaction Methods 0.000 claims abstract description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 239000000975 dye Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000000862 absorption spectrum Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 150000002505 iron Chemical class 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- PKIFBGYEEVFWTJ-UHFFFAOYSA-N hexaphene Chemical compound C1=CC=C2C=C3C4=CC5=CC6=CC=CC=C6C=C5C=C4C=CC3=CC2=C1 PKIFBGYEEVFWTJ-UHFFFAOYSA-N 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- LHOWRPZTCLUDOI-UHFFFAOYSA-K iron(3+);triperchlorate Chemical compound [Fe+3].[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O.[O-]Cl(=O)(=O)=O LHOWRPZTCLUDOI-UHFFFAOYSA-K 0.000 claims description 2
- 241000399119 Spio Species 0.000 claims 3
- 150000001412 amines Chemical class 0.000 claims 1
- 238000001514 detection method Methods 0.000 claims 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 10
- 239000002351 wastewater Substances 0.000 abstract description 6
- 239000000696 magnetic material Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000002122 magnetic nanoparticle Substances 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 239000003463 adsorbent Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- VYXSBFYARXAAKO-WTKGSRSZSA-N chembl402140 Chemical compound Cl.C1=2C=C(C)C(NCC)=CC=2OC2=C\C(=N/CC)C(C)=CC2=C1C1=CC=CC=C1C(=O)OCC VYXSBFYARXAAKO-WTKGSRSZSA-N 0.000 description 3
- 238000004043 dyeing Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 240000001973 Ficus microcarpa Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 230000004043 responsiveness Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 239000003011 anion exchange membrane Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000010291 electrical method Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WTFXARWRTYJXII-UHFFFAOYSA-N iron(2+);iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+2].[Fe+3].[Fe+3] WTFXARWRTYJXII-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of preparation method of magnetic graphene composite.The characteristics of on modified by magnetic nanoparticles to graphene nanometer sheet, it conveniently separates the high adsorption of graphene and magnetic material, is combined by the graphene composite material, forms a kind of new magnetic Nano biological adsorption material.This preparation method solves the shortcomings that grapheme material is easily reunited, and considerably increases the specific surface area of sorbing material, adds the binding site of sorbing material, expands absorption object range.Magnetic graphene composite material and preparation method thereof of the invention is simple, cost is cheap, physical and chemical performance is stable, reusable, and simple and easy ways and means is provided for environmental wastewater processing and waste reclamation.
Description
Technical field
The invention belongs to field of nanometer technology and biological adsorption field, and in particular to a kind of magnetic graphene composite
Preparation method, the composite nano materials have superparamagnetism and stronger absorption property, can be used as a kind of new biological adsorption
Material is used for the absorption of organic dyestuff.
Background technology
With flourishing for industry, waste water pollution problem is increasingly serious.Wherein heavy metal wastewater thereby and organic wastewater yield
Big and its complicated component, harm is huge, and how to carry out efficient processing is the focus studied at present.
The organic dyestuff administering method being reported at present has：（1）Pass through the anion-exchange membrane of Inorganic whisker
Remove anionic dye；（2）Organic matter is flocculated using polyaluminium chloride；（3）Photocatalytic degradation is used for organic dyestuff；（4）
Traditional electrical method is instead of using electro multiphase catalysis to give up to handle dyestuff；（5）Absorption method.Wherein, absorption method using new or
The material that person discards will greatly save process costs, obtain higher benefit, at present as organic matter processing as adsorbent
Study hotspot.For different Adsorption objects and adsorbent, the mechanism to interact between the two is not quite similar, main
Active force has molecular force effect, electrostatic force, pi-electron rail effect, ion exchange, surface complexation, redox and thin
Hole absorption etc..
For graphene oxide as a kind of new nano adsorption material, itself has the specific surface area of super large and porous knot
Structure, chemical property is stable, and electric conductivity and absorption property are good, can be achieved to adsorb two kinds of materials completely different in waste water simultaneously,
Work well.It is small yet with graphene particle diameter, it is not easy to filter and precipitates, separation and recovery turns into the key of limitation graphene application
Problem, the quick separating of graphene oxide is realized there is an urgent need to seek a kind of easy-to-use method.Therefore, by graphene oxide
Assign magnetic behavior, it is possible to achieve efficiently separating between magnetic graphene adsorbent and waste water.Moreover, magnetic adsorbent application
There is the advantage of zero power consumption separation in Adsorption, under additional magnetic fields, short a few minutes can realizes that both are complete
Full separation.
The content of the invention
It is an object of the invention to provide a kind of magnetic graphene with big specific surface area and good magnetic responsiveness to answer
The preparation method of condensation material, composite Nano biological adsorption agent prepared by this method have strong magnetic responsiveness, strong adsorption force, prepare work
Skill is simple, good dispersion and the advantages that size uniform, has in field of nano biotechnology and biological adsorption field and widely should
With.
The present invention is achieved by the following measures：
A kind of preparation method of magnetic graphene composite, using following steps：
Trivalent iron salt, hexa and graphene oxide are dissolved in ethylene glycol solution, moved to after ultrasonic disperse
Hydro-thermal autoclave, reacted at 150 DEG C -220 DEG C 4-12 hours, room temperature is cooled to after reaction completely, with magnet by magnetic
Material is isolated from solution, is separated again with magnet after being washed repeatedly with water and organic solvent, then by isolated magnetic
Material is dried, and finally obtains magnetic graphene composite.
Trivalent iron salt of the present invention is one kind in iron chloride, ferric sulfate, ferric nitrate, ferric perchlorate or ironic citrate；
The trivalent iron salt, hexa, the amount ratio of graphene oxide and ethylene glycol are 0.1-0.5g：0.2-1.5g：0.2-
2g：10-100mL；The ultrasonic disperse time is 10-90min.
Organic solvent of the present invention is absolute ethyl alcohol or acetone；Drying temperature is 50-100 DEG C, drying time 1-
10h。
The present invention can be used as a kind of efficient organic dye adsorbent namely, and magnetic graphene composite, which is added, engine dyeing
10-120min is stirred in material solution, after reaction completely, is isolated magnetic graphene composite nanometer particle from solution with magnet
Come, the content of remaining organic dyestuff in solution is detected by ultra-violet absorption spectrum；The wherein concentration of magnetic graphene composite
For 0.5-2.5 g/L, the concentration of organic dyestuff is 1 × 10-6-1×10-4 mol/L。
Beneficial effects of the present invention：
（1）Magnetic graphene composite is while performance graphene peculiar advantage, by introducing the oxidation of magnetic four three
Iron realizes the functionalization to grapheme material, further expands the application field of grapheme material, while overcomes graphene certainly
Body is easily accumulated, the shortcomings that bad dispersibility；
（2）Graphene provided by the invention adds magnetic method of modifying, and technique is simple, and preparation condition is gentle, and cost is cheap；
（3）Magnetic graphene composite provided by the invention can be used for field of waste water treatment.
Brief description of the drawings
Fig. 1 is the Raman spectrogram of magnetic graphene composite
Fig. 2 is the abosrption spectrogram that magnetic graphene composite adds different time after rhodamine 6G
Fig. 3 is the XRD spectrum of magnetic graphene composite
Fig. 4 is to add different amounts of magnetic graphene composite in rhodamine B solution to adsorb the absorption spectrum after 90min
Figure
Fig. 5 is the TEM collection of illustrative plates of magnetic graphene composite.
Embodiment
Illustrate technical scheme below by specific embodiment, but technical scheme is not with specific real
Example is applied to be limited.
Embodiment 1：
0.1g ferric chloride hexahydrates, 0.3g hexas and 0.5g graphene oxides are dissolved in 50mL ethylene glycol solutions
In, hydro-thermal autoclave is moved to after 30min ultrasonic disperses, is reacted 8 hours at 150 DEG C, room is cooled to after reaction completely
Temperature, magnetisable material is isolated from solution with magnet, separated again with magnet after being washed repeatedly with water and absolute ethyl alcohol, then will
Isolated magnetic graphene dries 10h at 50 DEG C, finally obtains magnetic graphene composite.Fig. 1 is magnetic graphite
The Raman spectrogram of alkene composite.
Magnetic graphene composite is added in organic dyestuff rhodamine 6G solution and stirs 120min, after reaction completely,
Magnetic graphene composite nanometer particle is separated from solution with magnet, detected by ultra-violet absorption spectrum remaining in solution
The content of organic dyestuff；Wherein the concentration of magnetic graphene composite is 0.5 g/L, and the concentration of organic dyestuff is 1 × 10-6
mol/L.Fig. 2 is the abosrption spectrogram that magnetic graphene composite adds different time after rhodamine 6G.
Embodiment 2：
0.8g ferric sulfate, 1.1g hexas and 1g graphene oxides are dissolved in 70 mL ethylene glycol solutions, passed through
Hydro-thermal autoclave is moved to after 60min ultrasonic disperses, is reacted 6 hours at 180 DEG C, room temperature is cooled to after reaction completely, is used
Magnet isolates magnetisable material from solution, is separated again with magnet after being washed repeatedly with water and acetone, then will be isolated
Magnetic graphene at 80 DEG C dry 6 h, finally obtain magnetic graphene composite.Fig. 3 is magnetic graphene composite wood
The XRD spectrum of material.
Magnetic graphene composite is added in organic dyestuff rhodamine B solution and stirs 90 min, after reaction completely, is used
Magnet separates magnetic graphene composite nanometer particle from solution, and detecting residue in solution by ultra-violet absorption spectrum has
The content of engine dyeing material；Wherein the concentration of magnetic graphene composite is 2 g/L, and the concentration of organic dyestuff is 1 × 10-5 mol/
L.Fig. 4 is to add different amounts of magnetic graphene composite in rhodamine B solution to adsorb the abosrption spectrogram after 90min.
Embodiment 3：
1.2 g ferric nitrates, 1.8 g hexas and 1.5 g graphene oxides are dissolved in 100 mL ethylene glycol solutions
In, hydro-thermal autoclave is moved to after 90min ultrasonic disperses, is reacted 6 hours at 200 DEG C, room is cooled to after reaction completely
Temperature, magnetisable material is isolated from solution with magnet, separated again with magnet after being washed repeatedly with water and absolute ethyl alcohol, then will
Isolated magnetic graphene dries 4 h at 100 DEG C, finally obtains magnetic graphene composite.Fig. 5 is magnetic stone
The TEM collection of illustrative plates of black alkene composite.
Magnetic graphene composite is added in organic dyestuff rhodamine B solution and stirs 90 min, after reaction completely, is used
Magnet separates magnetic graphene composite nanometer particle from solution, and detecting residue in solution by ultra-violet absorption spectrum has
The content of engine dyeing material；Wherein the concentration of magnetic graphene composite is 2.5 g/L, and the concentration of organic dyestuff is 1 × 10-4
mol/L。
Claims (4)
1. a kind of preparation method of magnetic graphene composite, it is characterised in that the magnetic graphene composite is by stone
Black alkene and SPIO composition, SPIO are uniformly distributed in graphite
The surface of alkene material, wherein SPIO particle diameter are 10-100nm；
Described preparation method comprises the following steps：
Trivalent iron salt, hexa and graphene oxide are dissolved in ethylene glycol solution, hydro-thermal is moved to after ultrasonic disperse
Autoclave, reacted at 150 DEG C -220 DEG C 4-12 hours, room temperature is cooled to after reaction completely, with magnet by magnetisable material
Isolate from solution, separated again with magnet after being washed repeatedly with water and organic solvent, then by isolated magnetisable material
Dry, finally obtain magnetic graphene composite.
A kind of 2. preparation method of magnetic graphene composite according to claim 1, it is characterised in that the trivalent
Molysite is one kind in iron chloride, ferric sulfate, ferric nitrate, ferric perchlorate or ironic citrate；The trivalent iron salt, hexa-methylene four
The amount ratio of amine, graphene oxide and ethylene glycol is 0.1-0.5g：0.2-1.5g：0.2-2g：10-100mL；The ultrasonic disperse time
For 10-90min.
3. the preparation method of a kind of magnetic graphene composite according to claim 1, it is characterised in that described has
Solvent is absolute ethyl alcohol or acetone；Drying temperature is 50-100 DEG C, drying time 1-10h.
A kind of 4. magnetic graphene composite answering in organic dyestuff absorption prepared by any methods describeds of claim 1-3
With, it is characterised in that：The magnetic graphene composite that in claim 1-3 prepared by any methods described is taken to add organic dyestuff
10-120min is stirred in solution, after reaction completely, is separated magnetic graphene composite from solution with magnet, is led to
Cross the content of remaining organic dyestuff in ultra-violet absorption spectrum detection solution；Wherein the concentration of magnetic graphene composite is 0.5-
2.5g/L, the concentration of organic dyestuff is 1 × 10-6-1×10-4mol/L。
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| CN106268950B (en) * | 2016-07-26 | 2018-09-28 | 扬州大学 | Has the preparation method of magnetic heteropoly acid-graphene composite catalyzing material |
| CN106186158A (en) * | 2016-08-01 | 2016-12-07 | 镇江市高等专科学校 | Two selenizing molybdenums/ferroferric oxide magnetic nano composite, Preparation Method And The Use |
| CN107252685B (en) * | 2017-06-19 | 2019-07-09 | 中南大学 | A kind of hydroxyl aminated compounds functional magnetic graphene oxide catalysis material and its preparation method and application |
| CN108212096B (en) * | 2017-12-30 | 2020-12-11 | 中国农业科学院油料作物研究所 | Fulvic acid modified magnetic graphene nanocomposite, preparation method and application |
| CN108722350B (en) * | 2018-05-07 | 2021-01-01 | 中国农业科学院油料作物研究所 | Magnetic graphene composite material and preparation method and application thereof |
| CN109019580A (en) * | 2018-09-27 | 2018-12-18 | 深圳天元羲王材料科技有限公司 | A kind of graphene purifying plant and method |
| CN110947950B (en) * | 2019-11-05 | 2021-08-24 | 中国船舶重工集团公司第七二五研究所 | Preparation method of graphene modified FeCo absorbent |
| CN110947369A (en) * | 2019-11-30 | 2020-04-03 | 河南永泽环境科技有限公司 | Preparation method and application of microalgae-based magnetic graphene and biochar |
| CN111569829B (en) * | 2020-04-15 | 2021-04-20 | 浙江省海洋水产研究所 | Method for removing micro-plastic in water based on graphene material |
| CN114288990B (en) * | 2021-12-29 | 2023-02-24 | 北京科技大学 | Preparation method of hydroxylated magnetic graphene oxide adsorbent |
| CN114797769A (en) * | 2022-03-30 | 2022-07-29 | 山东省花生研究所 | Application of magnetic graphene carbon nano material in aflatoxin adsorption |
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| CN103496693B (en) * | 2013-09-23 | 2015-04-29 | 郑州大学 | Method for preparing Fe3O4 nanoparticle/graphene composite material by sol electrostatic self-assembly process and application thereof |
| CN103594220A (en) * | 2013-11-21 | 2014-02-19 | 中国科学院长春应用化学研究所 | Functionalized grapheme/superparamagnetic ferroferric oxide nano particle composite material and preparation method thereof |
| CN104258810A (en) * | 2014-09-29 | 2015-01-07 | 扬州大学 | Adsorbing agent based on ferroferric oxide and graphene and preparation method of adsorbing agent |
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