CN111111691B - Nano-iron oxyhydroxide/metal/graphene ternary composite material and preparation method thereof - Google Patents
Nano-iron oxyhydroxide/metal/graphene ternary composite material and preparation method thereof Download PDFInfo
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- CN111111691B CN111111691B CN202010045006.6A CN202010045006A CN111111691B CN 111111691 B CN111111691 B CN 111111691B CN 202010045006 A CN202010045006 A CN 202010045006A CN 111111691 B CN111111691 B CN 111111691B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 66
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 title claims abstract description 44
- 239000011206 ternary composite Substances 0.000 title claims abstract description 36
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 23
- 239000002184 metal Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 42
- 239000010439 graphite Substances 0.000 claims description 42
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 37
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 23
- 229910052742 iron Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229910001510 metal chloride Inorganic materials 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 6
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000839 emulsion Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000006053 organic reaction Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 239000003381 stabilizer Substances 0.000 abstract 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 21
- 229910052763 palladium Inorganic materials 0.000 description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 238000004108 freeze drying Methods 0.000 description 6
- 238000001132 ultrasonic dispersion Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000002082 metal nanoparticle Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- 229910052707 ruthenium Inorganic materials 0.000 description 3
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 239000002127 nanobelt Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000002195 synergetic 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
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910002588 FeOOH Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- 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
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8906—Iron and noble metals
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a nano iron oxyhydroxide/metal/graphene ternary composite material and a preparation method thereof. The preparation method disclosed by the invention is simple in preparation process, no extra reducing agent or stabilizer is required to be added, the nano iron oxyhydroxide loaded on the graphene is in a strip shape and is uniformly distributed on the surface of the graphene, the wettability of the surface of the graphene is controllable, the operation process is simple, the production cost is low, the industrial production is easy to realize, and the obtained nano iron oxyhydroxide/metal/graphene ternary composite material has good amphipathy, is acid-base-resistant and high-temperature-resistant relative to graphene oxide, has high catalytic activity of metal species, and has potential application in two-phase organic reaction catalyzed by emulsion.
Description
Technical Field
The invention belongs to the technical field of preparation of nano composite materials, and particularly relates to a nano iron oxyhydroxide/metal/graphene ternary composite material and a preparation method thereof.
Background
The graphene material has the characteristics of large specific surface area, excellent physical properties, adjustable surface chemical properties and the like, and is concerned in recent years. Graphene oxide, which is an important member of a graphene family, shows good hydrophilicity due to the rich oxygen-containing functional groups, while the carbon of the main sheet layer makes the graphene oxide have certain hydrophobicity, and the performance of the graphene oxide is close to that of a two-dimensional surfactant, so that the graphene oxide already shows certain interfacial activity. However, the acid-base stability and the thermal stability of the graphene oxide are poor, so that the application of the graphene oxide in the aspect of interfacial catalysis organic chemical reaction is limited. The hydrophilic and hydrophobic solid particle hybridization synergistic effect can play a role in surface activity regulation, and the solid nanoparticles have more excellent thermal stability and acid and alkali stability compared with organic functional groups, so that a new idea is provided for graphene oxide interface regulation.
However, in the prior art, graphene is mainly used as a carrier material of a catalyst, and a metal nanoparticle is mainly supported by an immersion reduction method, a precipitation deposition method, or the like. In the reduction process of these methods, a liquid phase chemical reduction method using highly toxic hydrazine, hydrazine hydrate or the like as a reducing agent or a high temperature reduction method using a gas such as hydrogen, carbon monoxide or the like is generally used. The methods cannot effectively control the size, the dispersity and the loading amount of the loaded metal nanoparticles, and the loaded metal nanoparticles have poor binding force with a matrix, so that the interfacial activity of the surface of graphene is weakened, and the metal nanoparticles are easy to fall off from the matrix or agglomerate in the catalysis process, thereby reducing the catalytic activity. In fact, in these conventional methods, the biggest problem faced is that graphene is irreversibly agglomerated during the preparation process, and monodisperse graphene is not easily obtained; the interaction between the catalyst nanoparticles and the carrier is weak, graphene is difficult to be agglomerated together, and most of reported graphene sheets modified by the metal nanoparticles are in an aggregation state. Thus, the huge specific surface area of the graphene cannot be fully utilized, and the synergistic catalytic action of the compound cannot be fully exerted.
Disclosure of Invention
The invention aims to provide an acid-base-resistant and high-temperature-resistant nano iron oxyhydroxide/metal/graphene ternary composite material with good amphipathy and catalytic activity, and a simple preparation method for the ternary composite material, so that strip-shaped iron oxyhydroxide particles and metal are not coated by a surfactant and distributed on the surface of graphene in a monodisperse state, and the interfacial activity of the surface of the graphene is maintained.
Aiming at the purposes, the nano iron oxyhydroxide/metal/graphene ternary composite material adopted by the invention is prepared by the following method: ultrasonically dispersing graphite oxide in deionized water to obtain graphite oxide dispersion liquid; adding metal chloride into the graphite oxide dispersion liquid under the stirring condition, adding an organic solution containing iron pentacarbonyl, reacting for 1-3 hours under the closed condition at 50-80 ℃, filtering, washing and drying after the reaction is finished, thus obtaining the nano iron oxyhydroxide/metal/graphene ternary composite material.
In the above production method, the mass volume concentration of graphite oxide in the graphite oxide dispersion liquid is preferably 1 to 15mg/mL.
The metal chloride is any one of palladium chloride, nickel chloride and ruthenium chloride, the mass ratio of graphite oxide to metal chloride is preferably 5 to 1300, and the mass ratio of graphite oxide to metal chloride is more preferably 5 to 150.
In the above production method, the mass-to-volume ratio of graphite oxide to iron pentacarbonyl is preferably 0.01 to 5g, more preferably 0.03 to 1g.
In the organic solution containing iron pentacarbonyl, the volume concentration of the iron pentacarbonyl is preferably 1.5-135 mL/L.
The organic solution is any one of acetonitrile, acetone and benzaldehyde.
The invention has the following beneficial effects:
according to the invention, water and an organic solvent are simultaneously used as solvents, iron pentacarbonyl is used for reducing graphite oxide and metal chloride, no other reducing agent is added, and the nano-hydroxyl iron oxide/metal/graphene ternary composite material is prepared through a one-step reaction. The iron oxyhydroxide and the metal particles are loaded on the surface of the graphene in a nano-scale manner, the particle size is small, the iron oxyhydroxide and the metal particles are uniformly distributed on the surface of the graphene, and the stability and the dispersibility are good. The shape of the nano iron oxyhydroxide is a nano belt, and the nano belt is distributed on the surface of the graphene oxide in a monodisperse state. The method has the advantages of few synthesis steps, low production cost and easy realization of industrial production.
The nano iron oxyhydroxide/metal/graphene ternary composite material prepared by the invention has good amphipathy, and is acid-base-resistant and high-temperature-resistant compared with graphene oxide. And the surface wettability of the composite material can be regulated and controlled by regulating the proportion of the iron oxyhydroxide. Meanwhile, the composite material has metal species with high catalytic activity and has potential application in two-phase organic reaction catalyzed by emulsion.
Drawings
Fig. 1 is an XRD pattern of graphite oxide, nano-iron oxyhydroxide/palladium/graphene ternary composite material prepared in example 1, and an XRD standard card of iron oxyhydroxide.
Fig. 2 is a transmission electron microscope image of the nano iron oxyhydroxide/palladium/graphene ternary composite material prepared in example 1.
Fig. 3 is a contact angle of the nano iron oxyhydroxide/palladium/graphene ternary composite prepared in example 2 (a), example 3 (B), and example 4 (C).
FIG. 4 is a scanning electron microscope image of the ternary composite material of nano-iron oxyhydroxide/nickel/graphene prepared in example 5.
FIG. 5 is a transmission electron microscope image of the nano iron oxide hydroxide/nickel/graphene ternary composite material prepared in example 5.
Fig. 6 is a scanning electron microscope image of the nano iron oxyhydroxide/ruthenium/graphene ternary composite material prepared in example 6.
FIG. 7 is a transmission electron microscope image of the ternary composite material of nano-iron oxyhydroxide/ruthenium/graphene prepared in example 6.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Example 1
Adding 150mg of Graphite Oxide (GO) into 15mL of deionized water, and performing ultrasonic dispersion to obtain a graphite oxide dispersion liquid. Under the condition of stirring, adding 1mg of palladium chloride into the graphite oxide dispersion liquid, then transferring the graphite oxide dispersion liquid into a 150mL round-bottom flask, adding 15mL of acetonitrile solution with the volume concentration of 16.7mL/L of iron pentacarbonyl, reacting for 2 hours at 60 ℃ under the closed condition, filtering after the reaction is finished, washing with deionized water, and freeze-drying to obtain the nano iron oxyhydroxide/palladium/graphene ternary composite material (Pd/FeOOH @ RGO).
The XRD spectrum in figure 1 shows that the obtained product is a nano iron oxyhydroxide/palladium/graphene ternary composite material, figure 2 shows that the nano iron oxyhydroxide is in a strip shape, the width is about 15nm, the nano iron oxyhydroxide is dispersed on the surface of graphene, and the size of the nano palladium particle is about 5 nm.
Example 2
And adding 25mg of graphite oxide into 5mL of deionized water, and performing ultrasonic dispersion to obtain a graphite oxide dispersion liquid. Under the stirring condition, adding 5mg of palladium chloride into the graphite oxide dispersion liquid, then transferring the graphite oxide dispersion liquid into a 150mL round-bottom flask, adding 15mL of acetonitrile solution with the volume concentration of 5mL/L iron pentacarbonyl, reacting for 2 hours at 50 ℃ under the closed condition, filtering after the reaction is finished, washing with deionized water, and freeze-drying to obtain the nano iron oxyhydroxide/palladium/graphene ternary composite material.
Example 3
And adding 25mg of graphite oxide into 5mL of deionized water, and performing ultrasonic dispersion to obtain a graphite oxide dispersion liquid. Under the condition of stirring, adding 5mg of palladium chloride into the graphite oxide dispersion liquid, then transferring to a 150mL round-bottom flask, adding 15mL of acetonitrile solution with the volume concentration of 20mL/L iron pentacarbonyl, reacting for 2 hours at 50 ℃ under the closed condition, filtering after the reaction is finished, washing with deionized water, and freeze-drying to obtain the nano iron oxyhydroxide/palladium/graphene ternary composite material.
Example 4
And adding 25mg of graphite oxide into 5mL of deionized water, and performing ultrasonic dispersion to obtain a graphite oxide dispersion liquid. Under the stirring condition, adding 5mg of palladium chloride into the graphite oxide dispersion liquid, then transferring the graphite oxide dispersion liquid into a 150mL round-bottom flask, adding 15mL of acetonitrile solution with the volume concentration of 50mL/L iron pentacarbonyl, reacting for 2 hours at 50 ℃ under the closed condition, filtering after the reaction is finished, washing with deionized water, and freeze-drying to obtain the nano iron oxyhydroxide/palladium/graphene ternary composite material.
As can be seen from fig. 3, in examples 2, 3 and 4, the contact angle of the nano iron oxyhydroxide/palladium/graphene ternary composite material can be changed by controlling the concentration of the added iron pentacarbonyl, so as to change the wettability and surface activity of the composite material. With the increase of the concentration of the iron pentacarbonyl, the hydrophilicity of the composite material is reduced, and the lipophilicity is increased.
Example 5
Adding 125mg of graphite oxide into 15mL of deionized water, and performing ultrasonic dispersion to obtain a graphite oxide dispersion liquid; under the condition of stirring, adding 1mg of nickel chloride into the graphite oxide dispersion liquid, then transferring the graphite oxide dispersion liquid into a 150mL round-bottom flask, adding 15mL of acetonitrile solution with the volume concentration of 16.7mL/L of iron pentacarbonyl, reacting for 2 hours at 60 ℃ under the closed condition, filtering after the reaction is finished, washing with deionized water, and freeze-drying to obtain the nano iron oxyhydroxide/nickel/graphene ternary composite material. As can be seen from fig. 4 and 5, the composite material maintains the sheet structure of graphene, and the nano iron oxyhydroxide is in the form of a band and is dispersed on the surface of graphene.
Example 6
Adding 125mg of graphite oxide into 15mL of deionized water, and performing ultrasonic dispersion to obtain a graphite oxide dispersion liquid; under the condition of stirring, adding 1mg of ruthenium chloride into the graphite oxide dispersion liquid, then transferring the graphite oxide dispersion liquid into a 150mL round-bottom flask, adding 15mL of acetonitrile solution with the volume concentration of 16.7mL/L of iron pentacarbonyl, reacting for 2 hours at 60 ℃ under the closed condition, filtering after the reaction is finished, washing with deionized water, and freeze-drying to obtain the nano iron oxyhydroxide/ruthenium/graphene ternary composite material. As can be seen from fig. 6 and 7, the composite material maintains the sheet structure of graphene, and the nano iron oxyhydroxide is in the form of a band and is dispersed on the surface of graphene.
Claims (9)
1. A preparation method of a nano iron oxyhydroxide/metal/graphene ternary composite material is characterized by comprising the following steps: ultrasonically dispersing graphite oxide in deionized water to obtain graphite oxide dispersion liquid; adding metal chloride into the graphite oxide dispersion liquid under the stirring condition, adding an organic solution containing iron pentacarbonyl, reacting for 1-3 hours at 50-80 ℃ under a closed condition, filtering, washing and drying after the reaction is finished to obtain a nano iron oxyhydroxide/metal/graphene ternary composite material; the metal chloride is any one of palladium chloride, nickel chloride and ruthenium chloride.
2. The preparation method of the nano iron oxyhydroxide/metal/graphene ternary composite material according to claim 1, characterized in that: the mass volume concentration of the graphite oxide in the graphite oxide dispersion liquid is 1-15 mg/mL.
3. The preparation method of the nano iron oxyhydroxide/metal/graphene ternary composite material according to claim 1, characterized in that: the mass ratio of the graphite oxide to the metal chloride is 5-1300.
4. The preparation method of the nano iron oxyhydroxide/metal/graphene ternary composite material according to claim 3, characterized in that: the mass ratio of the graphite oxide to the metal chloride is 5-150.
5. The preparation method of the nano iron oxyhydroxide/metal/graphene ternary composite material according to claim 1, characterized in that: the mass volume ratio of the graphite oxide to the iron pentacarbonyl is 0.01-5 g.
6. The preparation method of the nano iron oxyhydroxide/metal/graphene ternary composite material according to claim 5, characterized in that: the mass volume ratio of the graphite oxide to the iron pentacarbonyl is 0.03-1 g.
7. The preparation method of the nano iron oxyhydroxide/metal/graphene ternary composite material according to claim 1, characterized in that: in the organic solution containing iron pentacarbonyl, the volume concentration of the iron pentacarbonyl is 1.5-135 mL/L.
8. The preparation method of the nano iron oxyhydroxide/metal/graphene ternary composite material according to claim 1, characterized in that: the organic solution is any one of acetonitrile, acetone and benzaldehyde.
9. The nano iron oxyhydroxide/metal/graphene ternary composite material prepared by the method of any one of claims 1 to 8.
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US5652192A (en) * | 1992-07-10 | 1997-07-29 | Battelle Memorial Institute | Catalyst material and method of making |
US7829140B1 (en) * | 2006-03-29 | 2010-11-09 | The Research Foundation Of The State University Of New York | Method of forming iron oxide core metal shell nanoparticles |
KR20150116489A (en) * | 2014-04-07 | 2015-10-16 | 인하대학교 산학협력단 | METHOD OF PREPARING IRON OXIDE-GRAPHENE COMPOSITES AND THE IRON OXIDE(β-FEOOH)-GRAPHENE COMPOSITES PREPARED BY THE SAME METHOD |
CN106082351A (en) * | 2016-06-01 | 2016-11-09 | 浙江大学 | The preparation method of a kind of FeOOH nanometer sheet and product thereof |
CN110152569A (en) * | 2018-04-28 | 2019-08-23 | 浙江大学 | A kind of nanometer Fe O (OH) composite aerogel, preparation method and use |
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US20130099153A1 (en) * | 2011-10-23 | 2013-04-25 | Postech Academy-Industry Foundation | Hybrid material comprising graphene and iron oxide, method for manufacturing the same, and apparatus for treating waste water using the same |
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US5652192A (en) * | 1992-07-10 | 1997-07-29 | Battelle Memorial Institute | Catalyst material and method of making |
US7829140B1 (en) * | 2006-03-29 | 2010-11-09 | The Research Foundation Of The State University Of New York | Method of forming iron oxide core metal shell nanoparticles |
KR20150116489A (en) * | 2014-04-07 | 2015-10-16 | 인하대학교 산학협력단 | METHOD OF PREPARING IRON OXIDE-GRAPHENE COMPOSITES AND THE IRON OXIDE(β-FEOOH)-GRAPHENE COMPOSITES PREPARED BY THE SAME METHOD |
CN106082351A (en) * | 2016-06-01 | 2016-11-09 | 浙江大学 | The preparation method of a kind of FeOOH nanometer sheet and product thereof |
CN110152569A (en) * | 2018-04-28 | 2019-08-23 | 浙江大学 | A kind of nanometer Fe O (OH) composite aerogel, preparation method and use |
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