CN111375410B - Preparation method of graphite alkynyl catalyst - Google Patents
Preparation method of graphite alkynyl catalyst Download PDFInfo
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- CN111375410B CN111375410B CN201811646311.XA CN201811646311A CN111375410B CN 111375410 B CN111375410 B CN 111375410B CN 201811646311 A CN201811646311 A CN 201811646311A CN 111375410 B CN111375410 B CN 111375410B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 52
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 43
- 239000010439 graphite Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000010949 copper Substances 0.000 claims abstract description 26
- 230000003197 catalytic effect Effects 0.000 claims abstract description 25
- -1 graphite alkyne Chemical class 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 7
- 150000001879 copper Chemical class 0.000 claims abstract description 6
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 239000002243 precursor Substances 0.000 claims abstract description 3
- 230000003647 oxidation Effects 0.000 claims description 14
- 238000007254 oxidation reaction Methods 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical group [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000000527 sonication Methods 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 8
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 abstract description 6
- 239000005751 Copper oxide Substances 0.000 abstract description 6
- 229910000431 copper oxide Inorganic materials 0.000 abstract description 6
- 230000010718 Oxidation Activity Effects 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000005470 impregnation Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 229910021389 graphene Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000003775 Density Functional Theory Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000011865 Pt-based catalyst Substances 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 description 1
- 238000006880 cross-coupling reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 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
- B01J23/72—Copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/864—Removing carbon monoxide or hydrocarbons
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20761—Copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/70—Non-metallic catalysts, additives or dopants
- B01D2255/702—Carbon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention discloses a preparation method of a graphite alkynyl catalyst, which comprises the following steps: adding the graphite alkyne powder into a precursor aqueous solution containing soluble copper salt, and uniformly dispersing the graphite alkyne powder by ultrasonic waves to obtain a dispersion liquid; drying the dispersion liquid at 50-80 ℃, and then calcining under the protection of inert gas, wherein the calcining temperature is 300-800 ℃. The invention creatively takes the graphyne as Cu x The copper oxide particles are successfully loaded on the surface of the graphite alkyne by the simple impregnation and calcination method of the carrier of O, the prepared catalyst has low-temperature catalytic oxidation activity on CO, the stability is not reduced due to long-time high-temperature test, and the economic benefit of the catalyst and the thermal stability of the catalyst are improved.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a graphite alkynyl catalyst, and more particularly relates to a preparation method of a graphite alkynyl CO catalytic oxidation catalyst.
Background
Graphyne (Graphdiyne) has immediately attracted considerable interest in the scientific community since its first synthesis in 2010 and has become one of the most popular materials in recent years. Graphyne is a novel allotrope of carbon with a two-dimensional structure and an intrinsic band gap sp - Hybridization is carried out. Compared to the allotrope family of carbon, graphynes consist of sp only - And sp 2- Hybridized carbon atom. The synthesis of graphdine promotes the research on the properties and applications of carbon materials. The unique structure and properties of graphdiyne make it exhibit many advantages in the fields of lithium storage materials, electrochemical actuators, battery electrode materials, hydrogen evolution and photocatalysis. At present, fundamental and applied research around graphdiynes has been actively conducted worldwide.
Graphdines not only have the characteristics of planar two-dimensional materials similar to graphene, but also have the characteristics of three-dimensional porous materials. Sp of graphathiane - And sp 2- The hybrid carbon network has a high degree of pi-conjugation and uniform distributionAnd tunable, enhanced electronic properties, are considered good candidates for non-metallic catalysts useful for low temperature catalytic oxidation of CO. To date in 2014, chenxin Cai et al successively proposed that graphyne can be used for catalytic oxidation of CO, and calculated the catalytic mechanism of graphyne and the catalyst of graphyne by a Density Functional Theory (DFT), but the preparation and application of such catalyst has never been reported experimentally so far. Therefore, it is of great significance to develop a method for preparing a catalyst for catalytic oxidation of CO from graphite alkynyl.
Many noble metals have been demonstrated to have high catalytic oxidation activity for CO, such as Au and Pt-based catalysts. However, how to effectively improve the activity of the catalyst for catalytic oxidation of CO and improve the stability of the catalyst still remains one of the technical problems to be solved by those skilled in the art.
Disclosure of Invention
In view of the above-mentioned problems, it is an object of the present invention to provide a catalyst for catalytic oxidation of CO. The preparation method of the catalyst containing graphite alkynyl. In another aspect of the invention, the invention also relates to the catalyst and the application thereof.
In order to solve the technical problem of the invention, the following technical scheme is adopted:
the invention relates to a preparation method of a graphite alkynyl catalyst, which is characterized by comprising the following steps:
adding the graphite alkyne powder into a precursor aqueous solution containing soluble copper salt, and uniformly dispersing the graphite alkyne powder by ultrasonic waves to obtain a dispersion liquid;
drying the dispersion liquid at 50-80 ℃, and then calcining under the protection of inert gas, wherein the calcining temperature is 300-800 ℃.
According to the invention, through ultrasonic treatment, the prepared graphite alkynyl catalyst can be prevented from being uneven in surface and agglomerated, so that the catalytic activity of the catalyst is influenced. In addition, the invention can decompose the soluble copper salt into Cu by calcining at 300-800 DEG C x O, also avoids decomposition of the graphdine itself.
In a preferred embodiment of the invention, the soluble copper salt is copper nitrate or a hydrate thereof.
In another preferred embodiment of the present invention, the time period of the ultrasonic treatment is 20 minutes or more.
In a preferred embodiment of the present invention, the drying time is 10 to 20 hours.
In a preferred embodiment of the present invention, the inert gas is selected from one or more of nitrogen or argon.
The invention also relates to the graphite alkynyl catalyst prepared by the preparation method and application thereof. For the graphite alkynyl catalyst of the invention, cu in the catalyst is Cu + And Cu 2+ The forms exist simultaneously. Preferably, the Cu + The ratio of Cu is about 25 to 30 mass%. By mixing Cu + The ratio of (b) is controlled within the preferable range of the present invention, and the catalytic activity and catalytic stability of the catalyst can be improved.
For the graphite alkynyl catalyst of the present invention, it is preferably used for the catalytic oxidation of CO. Particularly preferably, the catalytic oxidation is low-temperature catalytic oxidation, and the low-temperature catalytic oxidation means that the temperature of the catalytic reaction is 120 to 200 ℃.
Although the impregnation method is a common method for preparing the catalyst in the field, the invention creatively takes the graphdiyne as Cu x A carrier of O. Surprisingly, the copper oxide particles are successfully loaded on the surface of the graphite alkyne through a simple impregnation and calcination method, the prepared catalyst has low-temperature catalytic oxidation activity on CO, the stability is not reduced due to long-time high-temperature test, and the economic benefit of the catalyst and the thermal stability of the catalyst are improved.
Drawings
FIG. 1 is a scanning electron micrograph of a graphite alkynyl catalyst prepared in example 1;
FIG. 2 is a particle size distribution plot of the graphite alkynyl catalyst prepared in example 1;
FIG. 3 is a mapping chart of the graphite alkynyl catalyst prepared in example 1;
FIG. 4 is an XRD pattern of the graphite alkynyl catalyst prepared in example 1;
FIG. 5 is a Raman spectrum of the graphite alkynyl catalyst prepared in example 1;
FIG. 6 is an XPS spectrum of a graphite alkynyl catalyst prepared in example 1;
FIG. 7 is an XPS spectrum of a graphite alkynyl catalyst prepared in example 1;
FIG. 8 is a graph of the conversion efficiency of a catalyst catalyzing CO;
fig. 9 is a stability test chart of the catalyst.
Detailed Description
In order to further illustrate the technical solution of the present invention, the above technical solution is described in detail below with specific examples, but the present invention is not limited to the following embodiments.
Example 1:
according to the method recorded in the prior art, hexaalkynyl benzene is adopted to carry out cross coupling reaction under the catalytic action of a copper sheet, the graphite alkyne is prepared on the surface of the copper sheet, the obtained graphite alkyne powder is treated by acid and alkali with certain concentration, impurities such as Si, cu and the like are removed, and finally, the graphite alkyne powder is obtained by high-temperature calcination under the protection of inert atmosphere;
38mg of copper nitrate trihydrate are weighed and dissolved in 20ml of ethanol solution, and when the copper nitrate is completely dissolved, a certain amount of copper nitrate solution is weighed and added into a beaker weighing 100mg of graphite alkyne powder, so that the Cu/C mass ratio is 5%. Ultrasonically dispersing for 30min, transferring into a drying oven, drying at 60 deg.C for 12h, calcining the dried powder at 400 deg.C under protection of nitrogen atmosphere for 2h to obtain Cu x O/Graphdiyne catalyst, cu in the catalyst is Cu + And Cu 2+ Form (a) in which Cu is present + The proportion of the total Cu is about 25 to 30 mass%).
The relative characterization results for the graphite alkynyl catalyst prepared in example 1 are shown in fig. 1-7. Derivation of Cu from characterization results x The O/graphite alkynyl catalyst is successfully prepared. The scanning electron microscope result shows that the copper oxide is granular and evenly distributed on the surface of the graphite alkyne,the average particle size is 230nm. XRD, raman and XPS characterization results also further prove that Cu is contained x Successfully preparing the O/graphite alkynyl catalyst.
Catalytic oxidation activity of copper oxide/graphite alkyne, copper oxide/activated carbon, copper oxide/graphene CO test: 60000 ml of gas space velocity (s.v.) at atmospheric pressure using 80 mg of catalyst at a flow rate of 80 ml per minute and a gas space velocity (s.v.) per gram per hour in a 5mm diameter tubular quartz reactor. Gas from 1vol CO, 5vol% 2 And N 2 The composition of balance gas; the catalyst was heated from 30 ℃ to 250 ℃; the temperature was raised at a rate of 5 deg.C/s and then maintained for 30 minutes until the catalytic reaction reached a steady state. The stability test is carried out at 220 ℃,255 ℃ and 250 ℃, the test atmosphere and the activity test condition are kept consistent, and the test time is 24h.
The test results are shown in fig. 8 and 9. From FIG. 8, it can be seen that Cu x The O/graphite alkynyl catalyst shows the best catalytic oxidation activity and low-temperature activity. And from the stability test results shown in FIG. 9, cu x The O/graphite alkynyl catalyst shows better stability, while the comparative sample Cu x After 24h test, the activity of the O/active carbon is reduced by 70 percent, and the Cu content is reduced x The catalytic activity of O/graphene is reduced to almost 0%.
The applicant states that the present invention is described in detail by the above embodiments, but the present invention is not limited to the above embodiments, that is, the present invention is not limited to the above embodiments, and it should be understood by those skilled in the art that any modifications to the present invention, equivalent substitutions and additions to the present invention product, selection of specific modes, etc. are within the scope and disclosure of the present invention.
Claims (10)
1. The preparation method of the graphite alkynyl catalyst is characterized by comprising the following steps:
adding the graphite alkyne powder into a precursor aqueous solution containing soluble copper salt, and uniformly dispersing the graphite alkyne powder by ultrasonic waves to obtain a dispersion liquid;
drying the dispersion liquid at 50-80 ℃, and then calcining under the protection of inert gas, wherein the calcining temperature is 300-800 ℃.
2. The method according to claim 1, wherein the soluble copper salt is copper nitrate or a hydrate thereof.
3. The method according to claim 1, wherein the sonication is carried out for 20 minutes or longer.
4. The method according to claim 1, wherein the drying time is 10 to 20 hours.
5. The method according to claim 1, wherein the inert gas is selected from one or more of nitrogen and argon.
6. The graphite alkynyl catalyst prepared by the preparation method according to any one of claims 1 to 5.
7. The graphite alkynyl catalyst of claim 6, wherein Cu in the catalyst is Cu + And Cu 2+ The forms exist simultaneously.
8. The graphite alkynyl catalyst of claim 7, said Cu + The content of Cu is 25 to 30 mass%.
9. Use of the graphite alkynyl catalyst of any one of claims 6 to 8 for the catalytic oxidation of CO.
10. The use according to claim 9, wherein the catalytic oxidation is low-temperature catalytic oxidation, and the low-temperature catalytic oxidation refers to the temperature of catalytic reaction between 120 and 200 ℃.
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Non-Patent Citations (4)
| Title |
|---|
| Engineering the Coordination Environment of Single-Atom Platinum Anchored on Graphdiyne for Optimizing Electrocatalytic Hydrogen Evolution;Xue-Peng Yin等;《Angew. Chem. Int. Ed.》;20180628;第57卷;第9382–9386页 * |
| Graphdiyne-ZnO Nanohybrids as an Advanced Photocatalytic Material;Sakthivel Thangave等;《J. Phys. Chem. C》;20150828;第119卷;第22057-22065页 * |
| Graphyne-supported single Fe atom catalysts for CO oxidation;Ping Wu等;《Phys.Chem.Chem.Phys.》;20141020;第1441--1449页 * |
| Synthesis of Hierarchical Graphdiyne-Based Architecture for Efficient Solar Steam Generation;Xin Gao等;《Chem. Mater.》;20170627;第29卷;第5777-5781页 * |
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