CN114293217A - Preparation method of reduced graphene oxide composite metal nano array catalyst - Google Patents
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Abstract
The invention belongs to the technical field of catalyst preparation, and particularly relates to a preparation method of a reduced graphene oxide composite metal nano-array catalyst, which comprises the following steps: s1, dispersing graphene oxide in a medium to prepare a suspension, adding carbon cloth, and reacting at the temperature of 160-200 ℃ to prepare a carbon cloth precursor; s2, loading cobalt nitrate hexahydrate on the carbon cloth precursor prepared in the S1, and carrying out heat treatment at the temperature of 600 ℃ in the atmosphere of reducing gas to prepare the reduced graphene oxide composite metal nano array catalyst. The used raw materials are low in price, the preparation process is simple and safe, the period is short, the required equipment is simple, and the method is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of catalyst preparation, and particularly relates to a preparation method of a reduced graphene oxide composite metal nano-array catalyst.
Background
Along with the large consumption of fossil fuels, serious environmental problems and energy problems are brought, so that the development of clean, environment-friendly and renewable energy sources is urgent. Hydrogen energy has the advantages of high energy density, clean products, high combustion heat value, and the like, and is considered as an ideal substitute for the conventional fossil fuel. Among the preparation methods, the hydrogen production process by water electrolysis is simple, the product is clean, and the method is a way for obtaining high-efficiency hydrogen, but the reaction kinetics is slow, the potential is high, and the preparation process consumes extra energy, so the addition of the high-activity catalyst is critical. At present, the catalytic performance of noble metals is best, but its commercial use is hampered by its high price and low storage capacity. The non-noble metal catalyst with rich development resources, high efficiency and outstanding stability replaces noble metal, and large-scale production can be realized in the future. Carbon-based metal catalysts such as Co @ NC/NG, CoPs/NG, CoP @ NC/CF-900, NiFe/G, Co-P/N-dopedcarbonmates, Co @ N-CNTs @ rGO and the like have received much attention for their excellent catalytic properties.
The most widely used method is a chemical vapor deposition method, wherein cobalt chloride and Metal Organic Frameworks (MOFs) are used as raw materials, and a carbon-based metal catalyst is obtained through high-temperature calcination.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a reduced graphene oxide composite metal nano-array catalyst, which has the advantages of low price of used raw materials, simple and safe preparation process, short period, simple required equipment and suitability for large-scale production.
The invention is realized by the following technical scheme.
A preparation method of a reduced graphene oxide composite metal nano-array catalyst comprises the following steps:
s1, dispersing graphene oxide in a medium to prepare a suspension, adding carbon cloth, and reacting at the temperature of 160-200 ℃ to prepare a carbon cloth precursor;
s2, loading soluble cobalt salt on the carbon cloth precursor prepared in S1, and annealing at the temperature of 600 ℃ in the atmosphere of reducing gas to prepare the reduced graphene oxide composite metal nano array catalyst.
Preferably, in S1, the medium is a mixed solution of water and ethanol at a volume ratio of 1: 1.
Preferably, in S1, the usage ratio of the graphene oxide to the medium is 0.04 to 0.06 g: 30 ml.
Preferably, in S1, the carbon cloth is previously sonicated in nitric acid, then in water, and finally in ethanol.
Preferably, in S1, the reaction time is 10-15 h.
Preferably, in S2, the soluble cobalt salt is first dissolved in ethanol, then the S1 carbon cloth precursor is added, the ethanol is removed by heating, and after standing, the soluble cobalt salt is loaded on the carbon cloth precursor prepared in S1.
Preferably, in S2, the soluble cobalt salt is cobalt nitrate hexahydrate.
Preferably, the molar ratio of the graphene oxide to the soluble cobalt salt is 0.1-0.5: 1-5.
Preferably, in S2, the reducing gas is a hydrogen-argon mixture, and the flow rate is maintained at 100 mL/min.
Preferably, in S2, the temperature is increased from room temperature to 300-600 ℃ at a heating rate of 5 ℃/min, and the temperature is maintained for 1-6 h.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, firstly, graphene oxide and carbon cloth are subjected to hydrothermal treatment and then are dried at low temperature to obtain a precursor, then the precursor and a cobalt nitrate hexahydrate solution are mixed in a reducing gas atmosphere for annealing treatment, and the reduced graphene oxide composite metal nano array catalyst can be prepared by a hydrothermal-chemical vapor deposition two-step method;
2. the catalyst of the invention directly grows on the carbon cloth without using a polymer adhesive, thereby improving the conductivity; and the prepared product can be used for obtaining the reduced graphene oxide composite metal nano-array catalyst without washing with water, so that the operation process is simpler.
Drawings
FIG. 1 is a powder X-ray diffraction pattern of a reduced graphene oxide composite metal nanoarray catalyst as provided in example 1; FIG. 1b is an enlarged view of the upper left corner of FIG. a;
FIG. 2 is a graph of hydrogen evolution performance of a reduced graphene oxide composite metal nanoarray catalyst;
fig. 3 is an oxygen evolution performance diagram of a reduced graphene oxide composite metal nano-array catalyst.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to the following specific embodiments and the accompanying drawings, but the embodiments are not meant to limit the present invention.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
The invention provides a preparation method of a reduced graphene oxide composite metal nano-array catalyst, which comprises the following steps:
s1, dispersing graphene oxide in a medium to prepare a suspension, adding carbon cloth, and reacting at the temperature of 160-200 ℃ to prepare a carbon cloth precursor;
s2, loading soluble cobalt salt on the carbon cloth precursor prepared in S1, and annealing at the temperature of 600 ℃ in the atmosphere of reducing gas to prepare the reduced graphene oxide composite metal nano array catalyst.
In the method, metal Co is compounded with graphene oxide, and the metal is also suitable for Fe, Ni, Cu, Bi, W, Sn, In, Ce and Ga.
Example 1
A preparation method of a reduced graphene oxide composite metal nano-array catalyst comprises the following steps:
dissolving 0.05g of graphene oxide in 15mL of deionized water and 15mL of ethanol, stirring for 10min in a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out ultrasonic treatment for 30min to form a suspension, finally adding the treated carbon cloth (firstly, carrying out ultrasonic treatment for 30min in 3mol/L nitric acid solution, then carrying out ultrasonic treatment for 30min in deionized water, and finally carrying out ultrasonic treatment for 30min in ethanol), and reacting in an oven at 180 ℃ for 12 h; washing the obtained carbon cloth precursor with deionized water, and drying in a vacuum drying oven at 60 ℃ for 24 hours;
then, dissolving 0.441g of cobalt nitrate hexahydrate in 15mL of ethanol, adding a carbon cloth precursor after full dissolution, heating at 60 ℃ to remove a solvent, standing for 12 hours, putting the obtained pink carbon cloth sample and a porcelain boat into a quartz tube furnace, introducing 30min of hydrogen-argon mixed gas to remove air, and keeping the flow of the hydrogen-argon mixed gas at 100 mL/min; heating the tube furnace from room temperature to 450 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 4 h; and (3) after naturally cooling to room temperature, closing the hydrogen and argon mixed gas flow, and taking out the fired black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 2
A preparation method of a reduced graphene oxide composite metal nano-array catalyst comprises the following steps:
dissolving 0.05g of graphene oxide in 15mL of deionized water and 15mL of ethanol, stirring for 10min in a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out ultrasonic treatment for 30min to form a suspension, finally adding the treated carbon cloth (firstly, carrying out ultrasonic treatment for 30min in 3mol/L nitric acid solution, then carrying out ultrasonic treatment for 30min in deionized water, and finally carrying out ultrasonic treatment for 30min in ethanol), and reacting in an oven at 180 ℃ for 12 h; washing the obtained carbon cloth precursor with deionized water, and drying in a vacuum drying oven at 60 ℃ for 24 hours;
then, dissolving 0.441g of cobalt nitrate hexahydrate in 15mL of ethanol, adding a carbon cloth precursor after full dissolution, heating at 60 ℃ to remove a solvent, standing for 12 hours, putting the obtained pink carbon cloth sample and a porcelain boat into a quartz tube furnace, introducing 30min of hydrogen-argon mixed gas to remove air, and keeping the flow of the hydrogen-argon mixed gas at 100 mL/min; heating the tube furnace from room temperature to 500 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 4 h; and (3) after naturally cooling to room temperature, closing the hydrogen and argon mixed gas flow, and taking out the fired black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 3
A preparation method of a reduced graphene oxide composite metal nano-array catalyst comprises the following steps:
dissolving 0.05g of graphene oxide in 15mL of deionized water and 15mL of ethanol, stirring for 10min in a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out ultrasonic treatment for 30min to form a suspension, finally adding the treated carbon cloth (firstly, carrying out ultrasonic treatment for 30min in 3mol/L nitric acid solution, then carrying out ultrasonic treatment for 30min in deionized water, and finally carrying out ultrasonic treatment for 30min in ethanol), and reacting in an oven at 180 ℃ for 12 h; washing the obtained carbon cloth precursor with deionized water, and drying in a vacuum drying oven at 60 ℃ for 24 hours;
then, dissolving 0.441g of cobalt nitrate hexahydrate in 15mL of ethanol, adding a carbon cloth precursor after full dissolution, heating at 60 ℃ to remove a solvent, standing for 12 hours, putting the obtained pink carbon cloth sample and a porcelain boat into a quartz tube furnace, introducing 30min of hydrogen-argon mixed gas to remove air, and keeping the flow of the hydrogen-argon mixed gas at 100 mL/min; heating the tube furnace from room temperature to 400 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 4 h; and (3) after naturally cooling to room temperature, closing the hydrogen and argon mixed gas flow, and taking out the fired black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 4
A preparation method of a reduced graphene oxide composite metal nano-array catalyst comprises the following steps:
dissolving 0.05g of graphene oxide in 15mL of deionized water and 15mL of ethanol, stirring for 10min in a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out ultrasonic treatment for 30min to form a suspension, finally adding the treated carbon cloth (firstly, carrying out ultrasonic treatment for 30min in 3mol/L nitric acid solution, then carrying out ultrasonic treatment for 30min in deionized water, and finally carrying out ultrasonic treatment for 30min in ethanol), and reacting in an oven at 180 ℃ for 12 h; washing the obtained carbon cloth precursor with deionized water, and drying in a vacuum drying oven at 60 ℃ for 24 hours;
then, dissolving 0.294g of cobalt nitrate hexahydrate in 15mL of ethanol, adding a carbon cloth precursor after full dissolution, heating at 60 ℃ to remove the solvent, standing for 12 hours, putting the obtained pink carbon cloth sample and a porcelain boat into a quartz tube furnace, introducing 30min of hydrogen and argon mixed gas to remove air, and keeping the flow of the hydrogen and argon mixed gas at 100 mL/min; heating the tube furnace from room temperature to 450 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 4 h; and (3) after naturally cooling to room temperature, closing the hydrogen and argon mixed gas flow, and taking out the fired black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 5
A preparation method of a reduced graphene oxide composite metal nano-array catalyst comprises the following steps:
dissolving 0.05g of graphene oxide in 15mL of deionized water and 15mL of ethanol, stirring for 10min in a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out ultrasonic treatment for 30min to form a suspension, finally adding the treated carbon cloth (firstly, carrying out ultrasonic treatment for 30min in 3mol/L nitric acid solution, then carrying out ultrasonic treatment for 30min in deionized water, and finally carrying out ultrasonic treatment for 30min in ethanol), and reacting in an oven at 180 ℃ for 12 h; washing the obtained carbon cloth precursor with deionized water, and drying in a vacuum drying oven at 60 ℃ for 24 hours;
then, dissolving 0.147g of cobalt nitrate hexahydrate in 15mL of ethanol, adding a carbon cloth precursor after full dissolution, heating at 60 ℃ to remove the solvent, standing for 12 hours, putting the obtained pink carbon cloth sample and the porcelain boat into a quartz tube furnace, introducing 30min of hydrogen and argon mixed gas to remove air, and keeping the flow of the hydrogen and argon mixed gas at 100 mL/min; heating the tube furnace from room temperature to 450 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 4 h; and (3) after naturally cooling to room temperature, closing the hydrogen and argon mixed gas flow, and taking out the fired black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 6
A preparation method of a reduced graphene oxide composite metal nano-array catalyst comprises the following steps:
dissolving 0.05g of graphene oxide in 15mL of deionized water and 15mL of ethanol, stirring for 10min in a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out ultrasonic treatment for 30min to form a suspension, finally adding the treated carbon cloth (firstly, carrying out ultrasonic treatment for 30min in 3mol/L nitric acid solution, then carrying out ultrasonic treatment for 30min in deionized water, and finally carrying out ultrasonic treatment for 30min in ethanol), and reacting in an oven at 180 ℃ for 12 h; washing the obtained carbon cloth precursor with deionized water, and drying in a vacuum drying oven at 60 ℃ for 24 hours;
then, dissolving 0.588g of cobalt nitrate hexahydrate in 15mL of ethanol, adding a carbon cloth precursor after the cobalt nitrate hexahydrate is fully dissolved, heating at 60 ℃ to remove a solvent, standing for 12 hours, putting the obtained pink carbon cloth sample and a porcelain boat into a quartz tube furnace, introducing 30min of hydrogen and argon mixed gas to remove air, and keeping the flow of the hydrogen and argon mixed gas at 100 mL/min; heating the tube furnace from room temperature to 450 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 4 h; and (3) after naturally cooling to room temperature, closing the hydrogen and argon mixed gas flow, and taking out the fired black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 7
A preparation method of a reduced graphene oxide composite metal nano-array catalyst comprises the following steps:
dissolving 0.04g of graphene oxide in 15mL of deionized water and 15mL of ethanol, stirring for 10min in a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out ultrasonic treatment for 30min to form a suspension, finally adding treated carbon cloth (firstly, carrying out ultrasonic treatment for 30min in 3mol/L nitric acid solution, then carrying out ultrasonic treatment for 30min in deionized water, and finally carrying out ultrasonic treatment for 30min in ethanol), and reacting in an oven at 180 ℃ for 12 h; washing the obtained carbon cloth precursor with deionized water, and drying in a vacuum drying oven at 60 ℃ for 24 hours;
then, dissolving 0.441g of cobalt nitrate hexahydrate in 15mL of ethanol, adding a carbon cloth precursor after full dissolution, heating at 60 ℃ to remove a solvent, standing for 12 hours, putting the obtained pink carbon cloth sample and a porcelain boat into a quartz tube furnace, introducing 30min of hydrogen-argon mixed gas to remove air, and keeping the flow of the hydrogen-argon mixed gas at 100 mL/min; heating the tube furnace from room temperature to 450 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 4 h; and (3) after naturally cooling to room temperature, closing the hydrogen and argon mixed gas flow, and taking out the fired black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 8
A preparation method of a reduced graphene oxide composite metal nano-array catalyst comprises the following steps:
dissolving 0.06g of graphene oxide in 15mL of deionized water and 15mL of ethanol, stirring for 10min in a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, carrying out ultrasonic treatment for 30min to form a suspension, finally adding the treated carbon cloth (firstly, carrying out ultrasonic treatment for 30min in 3mol/L nitric acid solution, then carrying out ultrasonic treatment for 30min in deionized water, and finally carrying out ultrasonic treatment for 30min in ethanol), and reacting in an oven at 180 ℃ for 12 h; washing the obtained carbon cloth precursor with deionized water, and drying in a vacuum drying oven at 60 ℃ for 24 hours;
then, dissolving 0.441g of cobalt nitrate hexahydrate in 15mL of ethanol, adding a carbon cloth precursor after full dissolution, heating at 60 ℃ to remove a solvent, standing for 12 hours, putting the obtained pink carbon cloth sample and a porcelain boat into a quartz tube furnace, introducing 30min of hydrogen-argon mixed gas to remove air, and keeping the flow of the hydrogen-argon mixed gas at 100 mL/min; heating the tube furnace from room temperature to 450 ℃ at the heating rate of 5 ℃/min, and preserving the heat for 4 h; and (3) after naturally cooling to room temperature, closing the hydrogen and argon mixed gas flow, and taking out the fired black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Since the morphology and the performance of the reduced graphene oxide composite metal nano-array catalyst prepared in the above embodiment are basically the same, only the performance of the catalyst prepared in embodiment 1 will be described below. The catalyst obtained was subjected to X-ray diffraction, and the results are shown in FIG. 1. As can be seen from FIG. 1, XRD peak positions appeared at 44.8, 47.6 and 75.9 degrees corresponding to (002), (101) and (110) planes (PDF #05-0727), at 51.5 degrees corresponding to (200) plane (PDF #15-0806), and at 26.4 and 42.5 degrees corresponding to (002) and (100) planes (PDF #41-1487), indicating that the Co/RGO/CC catalyst was successfully prepared in this application.
The electrochemical performance of the prepared catalyst was measured, and the results are shown in fig. 2 and 3. As can be seen from FIG. 2, the current density of Co/RGO/CC in the alkaline solution was 10mA cm-2The hydrogen evolution overpotential required is 96 mV; as can be seen from FIG. 3, the current density of Co/RGO/CC in the alkaline solution was 10mA cm-2The required oxygen evolution overpotential is 301 mV; the catalyst prepared by the method has better catalytic performance.
It should be noted that when the following claims refer to numerical ranges, it should be understood that both ends of each numerical range and any value between the two ends can be selected, and since the steps and methods used are the same as those of the embodiments, the preferred embodiments of the present invention have been described for the purpose of preventing redundancy, but once the basic inventive concept is known, those skilled in the art may make other variations and modifications to the embodiments. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, it is intended that such changes and modifications be included within the scope of the appended claims and their equivalents.
Claims (10)
1. A preparation method of a reduced graphene oxide composite metal nano array catalyst is characterized by comprising the following steps:
s1, dispersing graphene oxide in a medium to prepare a suspension, adding carbon cloth, and reacting at the temperature of 160-200 ℃ to prepare a carbon cloth precursor;
s2, loading soluble cobalt salt on the carbon cloth precursor prepared in S1, and annealing at the temperature of 600 ℃ in the atmosphere of reducing gas to prepare the reduced graphene oxide composite metal nano array catalyst.
2. The method of claim 1, wherein in step S1, the medium is a mixture of water and ethanol at a volume ratio of 1: 1.
3. The method for preparing a reduced graphene oxide composite metal nano-array catalyst according to claim 1, wherein in S1, the dosage ratio of the graphene oxide to the medium is 0.04-0.06 g: 30 ml.
4. The method of preparing a reduced graphene oxide composite metal nano array catalyst according to claim 1, wherein in S1, the carbon cloth is previously subjected to ultrasonic treatment in nitric acid, then ultrasonic treatment in water, and finally ultrasonic treatment in ethanol.
5. The method for preparing a reduced graphene oxide composite metal nano-array catalyst according to claim 1, wherein in S1, the reaction time is 10-15 hours.
6. The method of claim 1, wherein in step S2, the soluble cobalt salt is first dissolved in ethanol, and then the S1 carbon cloth precursor is added, and the ethanol is removed by heating, and then the soluble cobalt salt is supported on the carbon cloth precursor prepared in step S1 after standing.
7. The method of claim 1, wherein in S2, the soluble cobalt salt is cobalt nitrate hexahydrate.
8. The method of claim 1, wherein the molar ratio of graphene oxide to soluble cobalt salt is 0.1-0.5: 1-5.
9. The method of claim 1, wherein in step S2, the reducing gas is a hydrogen-argon mixture, and the flow rate of the reducing gas is maintained at 100 mL/min.
10. The method as claimed in claim 1, wherein the step of S2 is carried out by heating from room temperature to 600 ℃ at a heating rate of 5 ℃/min and maintaining the temperature for 1-6 h.
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| CN110813293A (en) * | 2019-10-31 | 2020-02-21 | 曲阜师范大学 | Preparation method and application of Cu NPs-rGO electrocatalyst |
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