CN107243344A - A kind of one-step method for synthesizing of magnetic graphene - Google Patents
A kind of one-step method for synthesizing of magnetic graphene Download PDFInfo
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- CN107243344A CN107243344A CN201710331690.2A CN201710331690A CN107243344A CN 107243344 A CN107243344 A CN 107243344A CN 201710331690 A CN201710331690 A CN 201710331690A CN 107243344 A CN107243344 A CN 107243344A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000000661 sodium alginate Substances 0.000 claims abstract description 8
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 8
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 5
- 238000005119 centrifugation Methods 0.000 claims abstract description 5
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 235000010443 alginic acid Nutrition 0.000 claims 1
- 239000000783 alginic acid Substances 0.000 claims 1
- 229960001126 alginic acid Drugs 0.000 claims 1
- 229920000615 alginic acid Polymers 0.000 claims 1
- 150000004781 alginic acids Chemical class 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract description 19
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 238000006731 degradation reaction Methods 0.000 abstract description 10
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 4
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 230000003247 decreasing effect Effects 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B01J35/33—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
The invention discloses a kind of one-step method for synthesizing of magnetic graphene, comprise the following steps：(1) graphene oxide and Iron(III) chloride hexahydrate are made into the aqueous solution；(2) urea and sodium alginate are added, 200 DEG C of heating in reactor are subsequently transferred to, reaction is cooled to room temperature after terminating, products therefrom centrifugation, cleaning, dry after obtain the magnetic graphene.Obtain that pattern is homogeneous, magnetic graphene and the particle mean size only 7nm of even particle distribution.Resulting materials have excellent catalytic performance in the experiment of Photo Fenton system catalytic degradations methylene blue.In the environment of room temperature and weakly acidic pH (pH=6), 96% degradation rate can be reached after 120 minutes, hence it is evident that higher than Fe3O4Catalytic efficiency when making catalyst and degradation rate is recycled for multiple times has no and be decreased obviously, good catalytic performance can be similarly kept when being used in actual water sample.
Description
Technical field
The invention belongs to graphene synthesis technical field, and in particular to a kind of one-step method for synthesizing of magnetic graphene.
Background technology
With developing rapidly for science and technology, the living standard of people there occurs great variety.People are in developing industry and exploitation
While new energy, the problem of encountering new again is exactly environmental problem.How effectively to control discharge of wastewater and administer waste water into
One of major issue for facing mankind.Having been used for the technology of dye wastewater degradation has a lot, including chemical method, physico
Method, biological method or a variety of united methods, for example, charcoal absorption and microbial degradation etc..With homogeneous Fenton
The shortcomings of conventional waste water governance approach reacted for representative has catalyst hardly possible separation.The Fe grown up on this basis3O4
Though the heterogeneous Fenton oxidation for making catalyst utilizes Fe3O4Excellent magnetic property solves separation hardly possible, secondary pollution etc. well
Problem, but because of the unicity of material, still there is the drawbacks such as catalytic efficiency is low, applicable pH range is narrow.Research discovery, black light
Introducing with visible ray is greatly improved the speed of Fenton reactions, therefore Photo-Fenton methods have obtained extensive research,
Heterogeneous Photo-Fenton reactions especially by catalyst of carbon-based magnetic nanometer composite material not only can efficient removing waste
Organic dyestuff in liquid does not cause secondary pollution, and low energy consumption applicable pH range is wide, has good application prospect and high
Application value.
In addition, though environmental problem of the catalyst produced by is effectively solved, in catalyst synthesis processes
The environmental pollution brought by toxic reagent, such as use of hydrazine hydrate still can not be ignored.
The content of the invention
Present invention solves the technical problem that there is provided a kind of one-step synthesis magnetic graphene (RGO/Fe3O4) method, should
Method has obtained that pattern is homogeneous using large biological molecule sodium alginate as reducing agent and stabilizer, and particle is uniformly dispersed and Fe3O4Grain
Footpath only 7nm RGO/Fe3O4Composite, and the material Photo-Fenton systems degradation of methylene blue application in embody
More outstanding catalytic capability.
The present invention adopts the following technical scheme that method to solve above-mentioned technical problem,
A kind of one-step method for synthesizing of magnetic graphene, comprises the following steps：
(1) graphene oxide and Iron(III) chloride hexahydrate are made into the aqueous solution；
(2) urea and sodium alginate are added, 200C in reactor is subsequently transferred to and heats, reaction is cooled to room after terminating
Temperature, the magnetic graphene is obtained after products therefrom centrifugation, cleaning, drying.
Graphene oxide and the Iron(III) chloride hexahydrate mass ratio is 1: 15-20, preferably 1: 17.5.
The mass ratio of the urea and sodium alginate is 2-4: 1, preferably 2: 1.
200 DEG C of heat times are 10h in a kettle. for urea and sodium alginate.
Described cleaning is through water and absolute ethyl alcohol alternately cleaning 6 times by the product of centrifugation.
Described drying is to be dried in vacuo 7h at 60 DEG C.
The concentration of graphene oxide is 0.75-3.5mg/mL, the quality of the urea in the solution in described reaction solution
Concentration is 0.0125-0.05mg/mL.
Participation without any toxic reagent in present invention synthesis, condition is easily-controllable, easy to operate, environment-friendly, with synthesis
Equipment is simple, and raw material is common to be easy to get, the advantages of catalytic efficiency of quick and high efficient reaction and product is higher.
Brief description of the drawings
Fig. 1 is the synthetic route of magnetic graphene involved in the present invention；
Fig. 2 is graphene oxide (GO) made from the embodiment of the present invention 1, reduced graphene (RGO), RGO/Fe3O4With
Fe3O4XRD spectrum；
Fig. 3 is the transmission electron microscope collection of illustrative plates that magnetic graphene is made in the embodiment of the present invention 1.
Embodiment
The above to the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
It is the synthetic route of magnetic graphene involved in the present invention as shown in Figure 1.By the hydration trichlorines of 50mg GO and six
Change iron (FeCl3·6H2O) solid in mass ratio 1: 17.5 is made into the 10mL aqueous solution, and adding magnetic agitation 0.5h after 0.5g urea makes
Abundant dissolving, 21.2mM sodium alginate aqueous solution 30mL are added dropwise while stirring, be subsequently transferred in 50mL reactors 200 DEG C plus
Hot 10h.It is used for the Fe compareed in experiment3O4Nano particle is synthesized using identical method, and GO addition has simply been lacked in raw material,
And the RGO for being used to compare is to have lacked FeCl in raw material3·6H2O addition.
Fig. 2 is the XRD spectrum that material is made in the present embodiment, is graphene oxide (GO) successively from top to bottom, reduces graphite
Alkene (RGO), RGO/Fe3O4And Fe3O4XRD spectrum, bottom is Fe3O4Standard diagram (JCPDS card No.65-3107).
Diffraction maximum correspondence (001) crystal face that wherein GO occurs at 2 θ=10.8 °, the wide diffraction maximum pair that RGO occurs at 2 θ=23.0 °
(002) crystal face is answered, and from GO to RGO, the disappearance of (001) crystal face characteristic peak means GO with the appearance of (002) crystal face characteristic peak
Reduced by biomolecule sodium alginate to a certain extent.RGO/Fe3O4And Fe3O4Possess the diffraction maximum of same position, and
The Fe of bottom in the accurate corresponding diagram of energy3O4Standard diagram (JCPDS card No.65-3107), and RGO is in RGO/Fe3O4Figure
Obvious characteristic peak is not occurred in spectrum, reason is probably because its mass content is low and causes.
Fig. 3 is the transmission electron microscope collection of illustrative plates of magnetic graphene made from the present embodiment, wherein, figure (a-c) is different times magnifications
Shape appearance figure under rate, as seen from the figure Fe3O4Granular size is homogeneous and is evenly distributed, and figure (d) is lattice fringe figure, wherein between lattice
Away from for 0.296nm, correspondence Fe3O4(220) crystal face, figure (e) is selected diffraction, and diffraction ring is more obvious in figure, illustrates product
Crystallinity is good, wherein (331), (531), (422) crystal face are corresponding with XRD characterization results, (f) is schemed for granularmetric analysis figure, by scheming
Understand, Fe3O4Particle is smaller and average grain diameter only 7nm.
Using：
In 25 DEG C of room temperature, control time is 120min, and hydrogen peroxide initial concentration is 10.0mmolL-1, of methylene blue
Beginning concentration is 20mgL-1, RGO/Fe3O4Dosage is 0.25gL-1Under conditions of, the experiment bar that regulation solution starting pH is 6
Catalytic performance of the resulting materials in the experiment of Photo-Fenton system catalytic degradations methylene blue is probed under part.Experimental result table
It is bright, it can reach 96% degradation rate after 120min, and Fe3O4Make the degradation rate only 68.2% during catalyst, urge by contrast
Change efficiency and significantly improve and degradation rate is recycled for multiple times has no and be decreased obviously, can similarly be kept when being used in actual water sample
Good catalytic performance, there is very high application value and outstanding application prospect.
Embodiment above describes general principle, principal character and the advantage of the present invention, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (7)
1. a kind of one-step method for synthesizing of magnetic graphene, it is characterised in that comprise the following steps：
(1) graphene oxide and Iron(III) chloride hexahydrate are made into the aqueous solution；
(2) urea and sodium alginate are added, 200 DEG C of heating in reactor are subsequently transferred to, reaction is cooled to room temperature after terminating, institute
The magnetic graphene is obtained after obtaining product centrifugation, cleaning, drying.
2. a kind of one-step method for synthesizing of magnetic graphene according to claim 1, it is characterised in that：The graphite oxide
Alkene and Iron(III) chloride hexahydrate mass ratio are 1: 15-20.
3. a kind of one-step method for synthesizing of magnetic graphene according to claim 1, it is characterised in that：The urea and sea
The mass ratio of mosanom is 2-4: 1.
4. a kind of one-step method for synthesizing of magnetic graphene according to claim 1, it is characterised in that：Urea and alginic acid
200 DEG C of heat times are 10h to sodium in a kettle..
5. a kind of one-step method for synthesizing of magnetic graphene according to claim 1, it is characterised in that：Described cleaning is
By the product of centrifugation through water and absolute ethyl alcohol alternately cleaning 6 times.
6. a kind of one-step method for synthesizing of magnetic graphene according to claim 1, it is characterised in that：Described drying is
7h is dried in vacuo at 60 DEG C.
7. a kind of one-step method for synthesizing of magnetic graphene as claimed in claim 1, it is characterised in that：Stone is aoxidized in reaction solution
The concentration of black alkene is 0.75-3.5mg/mL, and the mass concentration of the urea is 0.0125-0.05mg/mL.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710331690.2A CN107243344B (en) | 2017-05-12 | 2017-05-12 | One-step synthesis method of magnetic graphene |
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| CN201710331690.2A CN107243344B (en) | 2017-05-12 | 2017-05-12 | One-step synthesis method of magnetic graphene |
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| Publication Number | Publication Date |
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| CN107243344B CN107243344B (en) | 2020-05-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110465293A (en) * | 2019-07-24 | 2019-11-19 | 北方工程设计研究院有限公司 | The preparation method and application of magnetic visible light heterogeneous Fenton catalyst |
| CN110563960A (en) * | 2019-09-16 | 2019-12-13 | 中国科学院生态环境研究中心 | Nitrogen-doped iron-based graphene gel, and preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110465293A (en) * | 2019-07-24 | 2019-11-19 | 北方工程设计研究院有限公司 | The preparation method and application of magnetic visible light heterogeneous Fenton catalyst |
| CN110563960A (en) * | 2019-09-16 | 2019-12-13 | 中国科学院生态环境研究中心 | Nitrogen-doped iron-based graphene gel, and preparation method and application thereof |
| CN110563960B (en) * | 2019-09-16 | 2021-04-02 | 中国科学院生态环境研究中心 | Nitrogen-doped iron-based graphene gel, and preparation method and application thereof |
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