CN109603831A - A kind of cobalt and graphene composite nano material catalyst and preparation method thereof - Google Patents
A kind of cobalt and graphene composite nano material catalyst and preparation method thereof Download PDFInfo
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- CN109603831A CN109603831A CN201811603520.6A CN201811603520A CN109603831A CN 109603831 A CN109603831 A CN 109603831A CN 201811603520 A CN201811603520 A CN 201811603520A CN 109603831 A CN109603831 A CN 109603831A
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- 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
- B01J23/75—Cobalt
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Abstract
The present invention relates to a kind of cobalts and graphene composite nano material catalyst and preparation method thereof.The main component of catalyst is cobalt and graphene；The preparation step of catalyst are as follows: loaded to cobalt salt from synthesis or commercially available redox graphene using infusion process, by drying after dipping, it obtains containing cobalt salt/graphene catalyst precursor, then presoma is roasted under nitrogen atmosphere, decompose cobalt salt, cobalt species and graphene are made to generate strong interaction simultaneously, cobalt and graphene composite nano material are obtained, which contains simultaneously combines closely monatomic cobalt, Cobalt cluster and cobalt/cobalt oxide nanoparticle with graphene-based bottom.
Description
Technical field
The present invention relates to a kind of cobalt and graphene composite nano material catalyst, the catalyst main component and this urge
The preparation method of agent.
Background technique
Excellent catalyst is the key that improve catalytic perfomance.The performance of catalyst is mainly determined by two aspects: one
It is ingredient, the other is preparation method.Same ingredient, using different preparation methods, performance can be widely different, similarly,
Same preparation method uses different ingredients, and can also tell on different catalyst.In recent years, containing monatomic, atom
The catalyst of cluster and the nanoparticle of even particle size distribution is increasingly taken seriously, and passes through the group in nano-level to catalyst
At, the regulation of structure and pattern and electronic state, efficient catalytic effect can be realized.Contain monoatomic catalyst preparation technology
Mainly including gradually reduction method (Zhang H., Kawashima K., Okumura M., et al.Colloidal Au
single-atom catalysts embedded on Pd nanoclusters[J].Journal ofMaterials
Chemistry A, 2014,2 (33): 13498.), infusion process (Mosesdebusk M., Yoon M., Allard L.F., et
al.CO oxidation on supported single Pt atoms:experimental and ab initio
density functional studies ofCO interaction with Pt atom onθ-Al2O3(010)
surface.[J].Journal ofthe American Chemical Society,2013,135(34):12634-
12645.), atomic layer deposition method (Xing J., Chen J.F., Li Y.H., et al.Stable Isolated Metal
Atoms as Active Sites for Photocatalytic Hydrogen Evolution[J].Chemistry-
AEuropean Journal, 2014,20 (8): 2138-2144.), anti-Ostward curing method (Hu, P., Huang, Z.,
Amghouz,Z.,Makkee,M.,Xu,F.,Kapteijn,F.,Dikhtiarenko,A.,Chen,Y.,Gu,X.and Tang,
X.(2014),Electronic Metal–Support Interactions in Single-Atom
Catalysts.Angew.Chem.Int.Ed., 53:3418-3421.) etc..Although it is negative that certain methods can obtain preferable metal
Effect is carried, but preparation process loads, it is at high cost, it is difficult to industrialization promotion.
From the point of view of catalyst component, graphene (graphene) is used as brand-new material, due to its unique substance
Structure and physicochemical property yield unusually brilliant results in catalytic field.By graphite powder using hummers method (William S.Hummers Jr,
Richard E.Offeman.Preparation ofGraphitic Oxide[J].Journal ofthe American
Chemical Society, 1958,80 (6): 1339.) being made graphene oxide (GO), then obtains being gone back by reduction again
Former graphene oxide (rGO) has the possibility produced in enormous quantities, this enables graphene as large catalyst preparation
Material.It is some the study found that metal is with nano particle (nanoparticles, NPs), cluster (clusters) or single former
The form of sub (single atoms) is present in graphene surface, under metal and graphene synergistic effect, can generate excellent
Catalytic effect.But the synthesis containing monoatomic catalyst acquires a certain degree of difficulty, and along with the hydrophobicity of grapheme material, makes
Metal Supported becomes more difficult.Currently, the method for carrying metal particles is mainly include the following types: the first side on graphene
Method, prefabricated NPs and graphene dispersion in a solvent, are interacted using electrostatic interaction or Van der Waals force and π-pi bond
Driving attachment.This method can preferably control the characteristic of NPs, but catalyst and unstable；Second method, allows target NPs
It is formed in situ on graphene-based material, functional group or the aromatic ring structure of graphene is made to stablize NPs.In this case,
The better interaction between NPs and carrier may be implemented, but the control to NPs structure and form may be lost；The
Three kinds of methods, the formation of metal/metal chemical combination object NPs and the conversion progress in situ simultaneously of GO to rGO, in this way can be with fortifying catalytic
Interaction between agent and metal component；Fourth method, NPs and graphene pass through a step from bottom to top by small molecule
Method is formed in situ, to synthesize catalyst (Das VK, the ShifrinaZ B, Bronstein of high stability
LM.Graphene and graphene-like materials in biomass conversion:paving the way
To the future [J] .Journal ofMaterials ChemistryA, 2017,5 (48)), this method is at high cost, item
Part is harsh, it is difficult to the extensive synthesis of industrialization.In addition, noble metal and transition-metal catalyst that the above method synthesizes,
Its metal and metal oxide exist generally in the form of NPs on carrier, and seldom occur monatomic, and metal is mostly
Use noble metal, and nontransition metal.It is seldom that the report on graphene is supported on about monatomic transition metal at present.(Deng
D,Chen X,LiangY,et al.A single iron site confined in a graphene matrix for
the catalytic oxidation of benzene at room temperature[J].Science Advances,
2015,1 (11): e1500462-e1500462. introduces FeN ingredient using graphene as carrier, with FePC, makes Fe in carrier
On in the form of monoatomic in conjunction with four N atoms, remarry and be connected on graphene carbon skeleton.(Fei,H.,Dong,J.,Feng,
Y.,Allen,C.S.,Wan,C.,Volosskiy,B.,et al.(2018).General synthesis and
definitive structural identification of MN4C4single-atom catalysts with
Tunable electrocatalytic activities.Nature Catalysis, 1 (1), 63-72) by Fe, Co, Ni chlorine
Salt is dried to obtain catalyst precursor after mixing hydrothermal treatment with graphene oxide, hydrogen peroxide, then catalyst precursor is existed
It is reacted in 900 DEG C of Ar air-flow with ammonia, obtains monatomic catalyst, M-NHGFs (M=Fe, Co, Ni), in such catalyst
Transition metal is connected by N atom with graphene, i.e., with MN4C4(M=Fe, Co, Ni) form exists, and the catalyst is in analysis oxygen electricity
There is good application effect in catalysis reaction.Up to the present, it there is no with dipping-roasting method on graphene synchronized loading list
The report of the catalyst of atom cobalt, Cobalt cluster and cobalt oxide nanoparticles ingredient.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art, the present invention will use a kind of simple method, i.e. dipping-roasting
Method synthesizes a kind of new catalyst containing variform cobalt on graphene, is named as Co/rGO.The catalyst is with transition
Metal Co is as active component, with redox graphene (rGO) for carrier, Co on carrier with many oxide (CoO,
Co2O3、Co3O4) nanoparticle, Co cluster and the presence of monatomic Co form.
The invention adopts the following technical scheme: a kind of cobalt-graphene composite nano material catalyst, main component is cobalt
And graphene, the carrying capacity of cobalt are as follows: cobalt accounts for 1~50wt% of catalyst quality；Preferably, the cobalt account for catalyst quality 5~
10wt%.Cobalt-graphene composite nano material catalyst preparation method is claimed simultaneously in the present invention, specifically includes following step
It is rapid:
(1) it impregnates
Cobalt salt is loaded on graphene using infusion process, by drying after dipping, is obtained containing cobalt salt/stone
The catalyst precursor of black alkene；
(2) it roasts
It will be roasted under nitrogen atmosphere in 400-700 DEG C containing cobalt salt/graphene catalyst precursor, make cobalt salt point
Solution, while cobalt and graphene being made to interact, obtain cobalt-graphene composite nano material catalyst.
The cobalt salt is that cobalt nitrate, cobalt acetate are one such or two kinds.
Cobalt salt solution first is configured using ethanol water in the step (1), wherein the content of ethyl alcohol is 10-80%, excellent
Choosing uses 20%.
The infusion process that the step (1) uses can be incipient impregnation, excessive dipping, preferentially use incipient impregnation.
In the step (2), roasting protective gas is the high pure nitrogen that purity reaches 99.95% or more.
In the step (2), maturing temperature is preferably 500-600 DEG C.
The present invention has the following advantages compared with the prior art and effect:
Present invention employs cheap transiting state metal cobalts as catalyst activity component, with simple incipient impregnation and roasting
Burning method has been prepared simultaneously containing combining closely monatomic cobalt, Cobalt cluster and cobalt/cobalt oxide nanoparticle with graphene-based bottom
Catalyst.
Detailed description of the invention
Fig. 1 HAADF-STEM characterization and monatomic Co simulation.
Specific embodiment
Below with reference to characterization and the embodiment of test reaction, the present invention is described in further detail, but of the invention
Embodiment is without being limited thereto.
Used graphene can be using synthesis or commercially available redox graphene (reduced certainly
Graphene oxide, rGO, abbreviation graphene)；The redox graphene (rGO) of synthetic catalyst is used in the present embodiment,
Abbreviation graphene can use commercialized graphene, can also be synthesized certainly according to Hummers method.RGO in this example
It is from synthesis, detailed step are as follows: take dry 2.0L beaker, the 230mL concentrated sulfuric acid and 5.0g sodium nitrate (NaNO is added3), it sets
It is stirred under ice bath, when temperature T≤5 DEG C, 10.0g natural flake graphite powder is added, continues stirring 2.5 hours；It is uniformly mixed
Afterwards, it is slowly added to 30.0g potassium permanganate (KMnO4), during which control system temperature (subtracts not higher than 20 DEG C when i.e. temperature increases too fast
Slow filler rate reduces mixing speed and ice block cooling is added)；Then beaker is transferred in 35 DEG C of waters bath with thermostatic control, continues to stir
After mixing reaction 2.0 hours, 460mL deionized water is added；It takes out beaker to be placed in 98 DEG C of oil baths, reaching 98 DEG C to solution temperature is
Start timing, stirs 15 minutes；It is eventually adding 1.4L deionized water and terminates reaction, while 25mL hydrogen peroxide (30%H is added2O2),
It was found that solution has brownish black to become bright yellow and has metallic luster；It takes out beaker and is down to room temperature, be centrifuged, be washed with deionized
(pH ≈ 7) is transferred to brown reagent bottle and is sealed spare i.e. graphene oxide (GO) lotion after 8-10 times.Take the GO of 1g butt
(a certain amount of GO lotion being taken, by obtaining GO powder after drying and dehydrating, so that the concentration of GO lotion be calculated) is dispersed in
In 1000mL deionized water, it is ultrasonically treated 30min, in a still aging evening, is then transferred in round-bottomed flask and (only takes top brown
Solution, bottom black solution are undispersed graphite oxide, are given up), 30% ammonium hydroxide of 25mL and 80% hydrazine hydrate of 6mL is added,
After 2000rpm magnetic agitation lower 95 DEG C of waters reflux 3h, 80% hydrazine hydrate of 4mL is added the reaction was continued 30min, take out flask,
4% hydrochloric acid to dark solution generation black flocculent deposit is added dropwise and floats on liquid level, and solution becomes clear, takes out while hot
Filter is washed to not having ammonium hydroxide taste with hot water, is lyophilized, obtains loose rGO powder.It takes 100mg rGO in 50mL beaker, uses
100uL liquid-transfering gun sequentially adds deionized water into beaker, and continues to stir, until rGO water seepage in the pasty state, measures its water absorption
For 7mL/g.
1. catalyst preparation
Co/rGO catalyst, specific steps are prepared using incipient impregnation-roasting two-step method are as follows:
(1) it impregnates:
The preparation of salting liquid: Co (NO is taken3)2·6H22.1mL salting liquid is made with deionized water dissolving in O 0.3mmol；It will
The configured salting liquid of 2.1mL adds 0.6mL dehydrated alcohol, shakes up in 50mL beaker；300mg rGO is weighed, is quickly added
Enter into beaker, cover solution completely, at the same with glass bar in the direction of the clock persistently stirring 30min to powder in the pasty state；It will
Beaker is sealed with tinfoil, and dazzling, is placed in room temperature 4h, is subsequently placed in 50 DEG C of dry 12h in vacuum oven；
(5) it roasts:
Catalyst in beaker is taken out, is ground with agate mortar, it is made to become powder, the powdered samples of preparation are put into
In quartz ampoule, be placed in tube furnace under nitrogen atmosphere through 10 DEG C/min temperature programming by room temperature to 500 DEG C, it is permanent at 500 DEG C
Temperature roasting 2h, sample sealed storage is taken out when temperature is down to room temperature.
2. characterization result
Catalyst is characterized using angle of elevation annular dark field-scanning transmission electron microscope (HAADF-STEM): taking minimal amount of Co/rGO
By ultrasonic disperse in ethanol solution, it is put into instrument and tests after preparing sample with copper mesh grid.Characterization result is shown in Fig. 1, by
Fig. 1 can be seen that many Co oxide nano particles of the uniform load on rGO, and a large amount of Co cluster and monatomic Co.
The preferable specific embodiment of the above, only the invention, but the protection scope of the invention is not
It is confined to this, anyone skilled in the art is in the technical scope that the invention discloses, according to the present invention
The technical solution of creation and its inventive concept are subject to equivalent substitution or change, should all cover the invention protection scope it
It is interior.
Claims (9)
1. a kind of cobalt-graphene composite nano material catalyst, which is characterized in that its main component is cobalt and graphene, system
Preparation Method the following steps are included:
(1) it impregnates
Cobalt salt is loaded on graphene using infusion process, by drying after dipping, is obtained containing cobalt salt/graphene catalyst
Presoma；
(2) it roasts
It will be roasted under nitrogen atmosphere in 400-700 DEG C containing cobalt salt/graphene catalyst precursor, decompose cobalt salt, together
When so that cobalt and graphene is interacted, obtain cobalt-graphene composite nano material catalyst；
It is structurally characterized in that on catalyst simultaneously containing combining closely monatomic cobalt, Cobalt cluster and cobalt oxide with graphene-based bottom
Compound nanoparticle.
2. catalyst according to claim 1, which is characterized in that the cobalt accounts for 5~10wt% of catalyst quality.
3. catalyst according to claim 1, which is characterized in that the cobalt salt is cobalt nitrate, cobalt acetate is one such
Or two kinds.
4. catalyst according to claim 1, which is characterized in that first configured using ethanol water in the step (1)
Cobalt salt solution, wherein the content of ethyl alcohol is 10-80%.
5. catalyst according to claim 4, which is characterized in that the content of ethyl alcohol is 20%.
6. catalyst according to claim 1, which is characterized in that the infusion process that the step (1) uses is to soak in equal volume
Stain or excessive infusion process.
7. catalyst according to claim 6, which is characterized in that use equi-volume impregnating.
8. catalyst according to claim 1, which is characterized in that in the step (2), roasting protective gas reaches for purity
To 99.95% or more high pure nitrogen.
9. catalyst according to claim 1, which is characterized in that in the step (2), maturing temperature is 500-600 DEG C.
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| CN111020625A (en) * | 2019-11-17 | 2020-04-17 | 塞文科技(上海)有限公司 | Phosphorus-doped graphene nanoribbon loaded cobalt monoatomic catalyst and preparation method thereof |
| CN112774690A (en) * | 2019-11-04 | 2021-05-11 | 北京氦舶科技有限责任公司 | Supported monatomic noble metal catalyst and preparation method and application thereof |
| CN113122878A (en) * | 2021-04-16 | 2021-07-16 | 陕西科技大学 | Nitrogen-doped carbon composite graphene coated metal cobalt catalyst, preparation method and application |
| CN113198463A (en) * | 2021-04-14 | 2021-08-03 | 云南大学 | Method for loading metal monoatomic atoms on surface of carbon material |
| CN113828317A (en) * | 2021-09-26 | 2021-12-24 | 大连大学 | Method for preparing metal monoatomic-graphene composite material |
| CN113996325A (en) * | 2021-10-21 | 2022-02-01 | 常州大学 | Nitrogen-doped graphene copper-based bimetallic monatomic catalyst and preparation method and application thereof |
| CN116037190A (en) * | 2023-01-31 | 2023-05-02 | 温州大学 | Transition metal cobalt-loaded graphene three-dimensional macroscopic catalyst, preparation method and application |
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| CN113122878A (en) * | 2021-04-16 | 2021-07-16 | 陕西科技大学 | Nitrogen-doped carbon composite graphene coated metal cobalt catalyst, preparation method and application |
| CN113828317A (en) * | 2021-09-26 | 2021-12-24 | 大连大学 | Method for preparing metal monoatomic-graphene composite material |
| CN113996325A (en) * | 2021-10-21 | 2022-02-01 | 常州大学 | Nitrogen-doped graphene copper-based bimetallic monatomic catalyst and preparation method and application thereof |
| CN113996325B (en) * | 2021-10-21 | 2022-07-01 | 常州大学 | Nitrogen-doped graphene copper-based bimetallic monatomic catalyst and preparation method and application thereof |
| CN116037190A (en) * | 2023-01-31 | 2023-05-02 | 温州大学 | Transition metal cobalt-loaded graphene three-dimensional macroscopic catalyst, preparation method and application |
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