CN108404989A - A kind of preparation method of Aurum clusters/graphene catalytic membrane - Google Patents
A kind of preparation method of Aurum clusters/graphene catalytic membrane Download PDFInfo
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- CN108404989A CN108404989A CN201810400142.5A CN201810400142A CN108404989A CN 108404989 A CN108404989 A CN 108404989A CN 201810400142 A CN201810400142 A CN 201810400142A CN 108404989 A CN108404989 A CN 108404989A
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical class [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 49
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 48
- 239000012528 membrane Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 210000004379 membrane Anatomy 0.000 claims abstract description 33
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003446 ligand Substances 0.000 claims abstract description 17
- 230000004224 protection Effects 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 230000009467 reduction Effects 0.000 claims abstract description 4
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 4
- 210000002469 basement membrane Anatomy 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 3
- 239000012498 ultrapure water Substances 0.000 claims abstract description 3
- 238000006722 reduction reaction Methods 0.000 claims description 8
- 239000000523 sample Substances 0.000 claims description 7
- 238000004108 freeze drying Methods 0.000 claims description 6
- GWOLZNVIRIHJHB-UHFFFAOYSA-N 11-mercaptoundecanoic acid Chemical class OC(=O)CCCCCCCCCCS GWOLZNVIRIHJHB-UHFFFAOYSA-N 0.000 claims description 3
- CMNQZZPAVNBESS-UHFFFAOYSA-N 6-sulfanylhexanoic acid Chemical group OC(=O)CCCCCS CMNQZZPAVNBESS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- LMJXSOYPAOSIPZ-UHFFFAOYSA-N 4-sulfanylbenzoic acid Chemical class OC(=O)C1=CC=C(S)C=C1 LMJXSOYPAOSIPZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims 2
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000012467 final product Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 description 11
- 239000000463 material Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000003643 water by type Substances 0.000 description 7
- 229910052737 gold Inorganic materials 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 238000003556 assay Methods 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000002242 deionisation method Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- FYEMIKRWWMYBFG-UHFFFAOYSA-N 8-sulfanyloctanoic acid Chemical compound OC(=O)CCCCCCCS FYEMIKRWWMYBFG-UHFFFAOYSA-N 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- GUWKQWHKSFBVAC-UHFFFAOYSA-N [C].[Au] Chemical class [C].[Au] GUWKQWHKSFBVAC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 239000012876 carrier material Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/226—Sulfur, e.g. thiocarbamates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/022—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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
- B01J35/59—Membranes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of preparation methods of Aurum clusters/graphene catalytic membrane, including：(1) deionized water is added into graphene oxide to be uniformly dispersed, ultrasonic disperse obtains dispersion liquid；Graphene oxide is reduced to by redox graphene rGO using hydrothermal reduction method, is freeze-dried, obtains rGO powders；(2) rGO powders are added in the Aurum clusters solution of mercaptan ligand protection, add ultra-pure water, ultrasonic disperse obtains mixed liquor；Mixed liquor is loaded on basement membrane using vacuum filtration, after washing to obtain the final product.The technology of the present invention is easy to operate, and Aurum clusters load capacity is big, and catalytic activity is high, easy to be recycled, realizes constructing for efficient catalytic film, has a good application prospect.
Description
Technical field
The invention belongs to catalytic membrane field, more particularly to the preparation method of a kind of Aurum clusters/graphene catalytic membrane.
Background technology
Recent studies indicate that catalytic process and membrane separating process are integrated in the same processing by catalytic separation film system
Unit has many advantages, such as that mass transfer is fast, easily amplification, process control and catalyst is recyclable.In addition, some catalytic separation films also have
Selectivity provides reactant, selective removal reaction product and accelerates the functions such as kinetics.To catalysis and separating property tool
There is core of the efficient membrane material of decisive role as this system, the pass of height has been inherently derived in catalytic separation film field
Note.But it prepares a kind of having both high catalytic activity, renewable, inexpensive, highly selective, high stability and green non-poisonous at this stage
Catalytic membrane is still one challenge of technical field of membrane.
On the one hand, the preparation of efficient stable catalytic membrane will also consider the micro- of material other than catalytic performance to be considered
See the influence of the properties such as pattern and surface characteristic.Carbon nanomaterial is due to having both superior electrical conductivity, high mechanical stability and big ratio
A kind of the features such as surface area, it is considered to be very promising catalytic separation film structure material.Wherein obtain the stone of extensive concern
Black alkene has the characteristics that large specific surface area and plane two-dimensional structure, is a kind of ideal catalyst support materials.But graphene has
Very strong hydrophobicity needs to realize in aqueous solution evenly dispersed by surfactant.In addition, grapheme material sheet
Body catalytic activity is extremely limited, but by Heteroatom doping or can load other catalyst and realize catalysis.
On the other hand, " dimensional effect " of noble metal nanometer material provides important opportunity for the development of catalytic separation film.
Gold nano cluster material has<The super-small of 2nm, shows the nanocrystal slightly larger with size and bulk is entirely different
" unusual dimensional effect ".But due to its extra small size, Aurum clusters are difficult to recycle from reaction solution.Therefore, Aurum clusters are improved
Stability and the repeatable Aurum clusters material utilized of exploitation are also a challenge of current catalytic field.
Invention content
Technical problem to be solved by the invention is to provide a kind of preparation method of Aurum clusters/graphene catalytic membrane,
This method technical operation is easy, and Aurum clusters load capacity is big, and catalytic activity is high, easy to be recycled, realizes the structure of efficient catalytic film
It builds, has a good application prospect.
The present invention provides a kind of preparation methods of Aurum clusters/graphene catalytic membrane, including：
(1) deionized water is added into graphene oxide to be uniformly dispersed, ultrasonic disperse obtains dispersion liquid；Using hydrothermal reduction
Graphene oxide is reduced to redox graphene rGO by method, and freeze-drying obtains rGO powders；
(2) the rGO powders in step (1) are added in the Aurum clusters solution of mercaptan ligand protection, are added ultrapure
Water, ultrasonic disperse obtain mixed liquor；Mixed liquor is loaded on basement membrane using vacuum filtration, Aurum clusters/graphite is obtained after washing
Alkene catalytic membrane；Wherein, the amount ratio of rGO and Aurum clusters is 5-10mg:5-20μmol.
Hydrothermal reduction reaction temperature in the step (1) is 120-200 DEG C, and the hydrothermal reduction reaction time is 3-20h.It is excellent
It is 5h to select the hydrothermal reduction reaction time.
A concentration of 1g/L-5g/L of dispersion liquid in the step (1).
Mercaptan ligand in the step (2) is 6- mercaptohexanoic acids (6-Mercaptohexanoic acid, MHA), 4- mercaptos
Yl benzoic acid (4-Mercaptobenzoic acid, MBA), 8- sulfydryls are sad (8-Mercaptooctanoic acid, MOA)
Or 11- Mercaptoundecanoic acids (11-Mercaptoundecanoic acid, MUA).
A concentration of 1mM of the Aurum clusters solution for having mercaptan ligand protection in the step (2).
Ultrasonic disperse in the step (1) and (2) is all made of Probe Ultrasonic Searching, ultrasonic power 50-500W, and ultrasonic time is
20-60min。
Washing in the step (2), which is adopted, to be washed with deionized.
The golden carbon atomic ratio of the Aurum clusters/graphene catalytic membrane obtained in the step (2) is 1%-6%, thickness
It is 5-20 μm.
The principle of the present invention is as follows：
It can be stabilized in aqueous solution due to the use of the gold nano cluster of mercaptan ligand protection, and the Aurum clusters
Mercaptan ligand can be combined with the hydrophobic grouping of graphene to promote graphene evenly dispersed in aqueous solution by hydrophobic effect.Gold
The mercaptan ligand of cluster plays the role of surfactant, and the gold atom of Aurum clusters plays the role of active site,
And graphene can be used as excellent carrier material realizes effective carrying of Aurum clusters, and the separation of cluster is contributed to return
It receives.Above-mentioned effect is expected to realize constructing for efficient catalytic film jointly.
Reduced graphene surface area is big, there is fold, is easy to chemical functional and modifies the payload, it can be achieved that Aurum clusters.And
Gold nano catalyst receives the favor of researcher, and successively developed a series of gold-carbon due to its efficient catalytic activity
Composite catalyzing material.Aurum clusters can promote the dispersion of graphene in water, graphene that can provide the work of attachment for Aurum clusters
Property site, the interaction of the two provide good basis for the preparation of composite membrane.Present invention demonstrates that the catalytic of composite membrane
It can be with the close relations such as the load capacity of the reducing degree of graphene and Aurum clusters.
Advantageous effect
The technology of the present invention is easy to operate, and Aurum clusters load capacity is big, and catalytic activity is high, easy to be recycled；Using mercaptan ligand
The Aurum clusters of protection not only can be to avoid reunion, but also the mercaptan ligands of Aurum clusters is utilized and is combined with the hydrophobic grouping of graphene to promote
Keep graphene evenly dispersed in aqueous solution, graphene is realized by the way of vacuum filtration and carries Aurum clusters, Aurum clusters
Gold atom plays the effect of active site, realizes constructing for efficient catalytic film, has a good application prospect.
Description of the drawings
Fig. 1 is the schematic diagram of Aurum clusters of the present invention/graphene catalytic membrane；
Fig. 2 is the pictorial diagram of Aurum clusters of the present invention/graphene catalytic membrane；
Fig. 3 is the electron scanning electron microscope (SEM) of Aurum clusters of the present invention/graphene catalytic membrane.
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, people in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
50mg graphene oxides are weighed in beaker with assay balance, and 25mL deionized waters are added and use Probe Ultrasonic Searching
15min is allowed to be uniformly dispersed, and obtains mixed liquor A, and A is poured into ptfe autoclave hydro-thermal 5h under conditions of 180 DEG C,
Obtained rGO be it is rodlike, taken after freeze-drying 5mg rGO be added 10mL mercaptan ligand protections Aurum clusters solution (1mM) and
10mL ultra-pure waters obtain finely dispersed mixed liquid B after ultrasonic 45min, B is smoked after film washed with 150mL deionizations it is extra
The catalytic membrane of homogeneous is formed after substance.With p-nitrophenol (4-NP) solution of 0.2mM flow velocity 1mL/min condition
The lower film 2h that crosses reaches the 0.5mM that degrades successively respectively after adsorption saturation, p-nitrophenol (4-NP) solution of 1.0mM, 1.5mM, drop
It is respectively 100%, 100%, 100% to solve effect.
Embodiment 2
50mg graphene oxides are weighed in beaker with assay balance, and 25mL deionized waters are added and use Probe Ultrasonic Searching
15min is allowed to be uniformly dispersed, and obtains mixed liquor A, and A is poured into ptfe autoclave hydro-thermal 5h under conditions of 180 DEG C,
Obtained rGO is rodlike, and 5mg rGO is taken to add the Aurum clusters solution (1mM) of 5mL mercaptan ligand protections and 15mL super after freeze-drying
Pure water obtains finely dispersed mixed liquid B after ultrasonic 45min, B is taken out after washing extra substance with 150mL deionizations after film
Form the catalytic membrane of homogeneous.Film is crossed under conditions of flow velocity 1mL/min with p-nitrophenol (4-NP) solution of 0.2mM
2h reaches the 0.5mM that degrades successively respectively after adsorption saturation, and the 4-NP solution of 1.0mM, 1.5mM, degradation effect is respectively 100%,
96.1%, 62.1%.
Embodiment 3
50mg graphene oxides are weighed in beaker with assay balance, and 25mL deionized waters are added and use Probe Ultrasonic Searching
15min is allowed to be uniformly dispersed, and obtains mixed liquor A, and A is poured into ptfe autoclave hydro-thermal 5h under conditions of 180 DEG C,
Obtained rGO is rodlike, and 5mg rGO is taken to add the Aurum clusters solution (1mM) of 20mL mercaptan ligand protections after freeze-drying, ultrasound
Finely dispersed mixed liquid B is obtained after 45min, and homogeneous is formed after washing extra substance with 150mL deionizations after B pumping films
Catalytic membrane.Film 2h is crossed under conditions of flow velocity 1mL/min reach absorption with p-nitrophenol (4-NP) solution of 0.2mM
Degrade 0.5mM successively respectively after saturation, 1.0mM, the 4-NP of 1.5mM, and degradation effect is respectively 100%, 100%, 100%.
Comparative example 1
50mg graphene oxides are weighed in beaker with assay balance, and 25mL deionized waters are added and use Probe Ultrasonic Searching
15min is allowed to be uniformly dispersed, which is poured into ptfe autoclave hydro-thermal 3h under conditions of 180 DEG C, is obtained
RGO be suspension, take 1/10th suspension be added 10mL mercaptan ligand protections Aurum clusters solution (1mM) and 10mL surpass
Pure water takes out film after ultrasonic 45min, and film is excessively fine and close, and water flux is too small.
Comparative example 2
50mg graphene oxides are weighed in beaker with assay balance, and 25mL deionized waters are added and use Probe Ultrasonic Searching
15min is allowed to be uniformly dispersed, and obtains mixed liquor A, and A is poured into ptfe autoclave hydro-thermal under conditions of 180 DEG C
10h, obtained rGO are rodlike, take 5mg rGO that the Aurum clusters solution (1mM) of 10mL mercaptan ligand protections is added after freeze-drying
With 10mL ultra-pure waters, not caning be uniformly dispersed after ultrasonic 45min (if increasing ultrasound intensity and ultrasonic time, theoretically can still divide
It dissipates).
Based on above example, the redox graphene after being handled by hydrothermal reduction being capable of abundant gold-supported group
Cluster, can be seen that prepared Aurum clusters/graphene catalytic membrane by the template reaction for p-nitrophenol of degrading has height
Catalytic activity, by further characterizing research (as shown in Figure 3), the Aurum clusters/graphene prepared under the conditions of described is compound to urge
The Aurum clusters changed in film are evenly distributed, and agglomeration does not occur.And compared to traditional batch-type, preparation method gained
Catalytic membrane can realize that continuous high-efficient is catalyzed, have preparation method simple, quickly, the features such as low energy consumption, non-secondary pollution.
Claims (8)
1. a kind of preparation method of Aurum clusters/graphene catalytic membrane, including：
(1) deionized water is added into graphene oxide to be uniformly dispersed, ultrasonic disperse obtains dispersion liquid；It will using hydrothermal reduction method
Graphene oxide is reduced to redox graphene rGO, and freeze-drying obtains rGO powders；
(2) the rGO powders in step (1) are added in the Aurum clusters solution of mercaptan ligand protection, add ultra-pure water, surpassed
Sound disperses to obtain mixed liquor；Mixed liquor is loaded on basement membrane using vacuum filtration, it is compound that Aurum clusters/graphene is obtained after washing
Catalytic membrane；Wherein, the amount ratio of rGO and Aurum clusters is 5-10mg:5-20μmol.
2. a kind of preparation method of Aurum clusters/graphene catalytic membrane according to claim 1, it is characterised in that：Institute
It is 120-200 DEG C to state the hydrothermal reduction reaction temperature in step (1), and the hydrothermal reduction reaction time is 3-20h.
3. a kind of preparation method of Aurum clusters/graphene catalytic membrane according to claim 1, it is characterised in that：Institute
State a concentration of 1g/L-5g/L of the dispersion liquid in step (1).
4. a kind of preparation method of Aurum clusters/graphene catalytic membrane according to claim 1, it is characterised in that：Institute
It is 6- mercaptohexanoic acids, 4- mercaptobenzoic acids, 8- sulfydryls octanoic acid or 11- Mercaptoundecanoic acids to state the mercaptan ligand in step (2).
5. a kind of preparation method of Aurum clusters/graphene catalytic membrane according to claim 1, it is characterised in that：Institute
State a concentration of 1mM of the Aurum clusters solution for having mercaptan ligand protection in step (2).
6. a kind of preparation method of Aurum clusters/graphene catalytic membrane according to claim 1, it is characterised in that：Institute
It states the ultrasonic disperse in step (1) and (2) and is all made of Probe Ultrasonic Searching, ultrasonic power 50-500W, ultrasonic time 20-60min.
7. a kind of preparation method of Aurum clusters/graphene catalytic membrane according to claim 1, it is characterised in that：Institute
It states the washing in step (2) and adopts and be washed with deionized.
8. a kind of preparation method of Aurum clusters/graphene catalytic membrane according to claim 1, it is characterised in that：Institute
The golden carbon atomic ratio for stating the Aurum clusters/graphene catalytic membrane obtained in step (2) is 1%-6%, and thickness is 5-20 μm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110261449A (en) * | 2019-05-15 | 2019-09-20 | 嘉兴鸿明传感科技有限公司 | A kind of preparation method and catalysis electrode of gas sensor catalysis electrode |
| CN111408366A (en) * | 2020-03-03 | 2020-07-14 | 合肥枡水新能源科技有限公司 | Preparation method of carbon-supported metal nanocluster catalyst |
| CN112023920A (en) * | 2020-08-03 | 2020-12-04 | 东华大学 | Preparation method and application of gold cluster-carbon nanotube electro-catalytic film |
| CN114210343A (en) * | 2022-01-24 | 2022-03-22 | 桂林电子科技大学 | Reduced graphene oxide loaded Ru-Ni bimetallic nanocluster catalytic material |
| CN115121244A (en) * | 2022-06-17 | 2022-09-30 | 武汉理工大学 | Method for preparing graphene-loaded gold cluster nanocomposite through in-situ reduction of sodium borohydride and application of graphene-loaded gold cluster nanocomposite |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010129385A (en) * | 2008-11-27 | 2010-06-10 | National Institute Of Advanced Industrial Science & Technology | Platinum cluster for electrode and method for producing the same |
| CN104227014A (en) * | 2014-09-18 | 2014-12-24 | 东南大学 | Method for preparing gold nano particle and graphene composite material through fast reduction |
| CN104841427A (en) * | 2015-04-24 | 2015-08-19 | 中国石油大学(北京) | GO/CNT-Au composite catalyst, preparation and application thereof |
-
2018
- 2018-04-28 CN CN201810400142.5A patent/CN108404989B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010129385A (en) * | 2008-11-27 | 2010-06-10 | National Institute Of Advanced Industrial Science & Technology | Platinum cluster for electrode and method for producing the same |
| CN104227014A (en) * | 2014-09-18 | 2014-12-24 | 东南大学 | Method for preparing gold nano particle and graphene composite material through fast reduction |
| CN104841427A (en) * | 2015-04-24 | 2015-08-19 | 中国石油大学(北京) | GO/CNT-Au composite catalyst, preparation and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| KYUJU KWAK ET AL: "Efficient Oxygen Reduction Electrocatalysts Based on Gold Nanocluster–Graphene Composites", 《CHEM. ELECTRO. CHEM.》 * |
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| CN110261449A (en) * | 2019-05-15 | 2019-09-20 | 嘉兴鸿明传感科技有限公司 | A kind of preparation method and catalysis electrode of gas sensor catalysis electrode |
| CN111408366A (en) * | 2020-03-03 | 2020-07-14 | 合肥枡水新能源科技有限公司 | Preparation method of carbon-supported metal nanocluster catalyst |
| CN112023920A (en) * | 2020-08-03 | 2020-12-04 | 东华大学 | Preparation method and application of gold cluster-carbon nanotube electro-catalytic film |
| CN114210343A (en) * | 2022-01-24 | 2022-03-22 | 桂林电子科技大学 | Reduced graphene oxide loaded Ru-Ni bimetallic nanocluster catalytic material |
| CN115121244A (en) * | 2022-06-17 | 2022-09-30 | 武汉理工大学 | Method for preparing graphene-loaded gold cluster nanocomposite through in-situ reduction of sodium borohydride and application of graphene-loaded gold cluster nanocomposite |
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