CN114293217B - Preparation method of reduced graphene oxide composite metal nano-array catalyst - Google Patents
Preparation method of reduced graphene oxide composite metal nano-array catalyst Download PDFInfo
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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 160-200 ℃ to prepare a carbon cloth precursor; s2, loading cobalt nitrate hexahydrate on the carbon cloth precursor prepared in the step S1, and performing heat treatment at 300-600 ℃ in a reducing gas atmosphere to prepare the reduced graphene oxide composite metal nano array catalyst. The raw materials used 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 massive consumption of fossil fuels, serious environmental problems and energy problems are brought along with the consumption of fossil fuels, so that the development of clean, environment-friendly and renewable energy sources is forced to be carried out at the eyebrows. The 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 traditional fossil fuel. In a plurality of preparation methods, the water electrolysis hydrogen production process 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 required to be high, and the preparation process consumes additional energy, so the addition of the high-activity catalyst is critical. At present, the catalytic performance of noble metals is the best, but the commercial application is hindered due to the high price and the low storage capacity. The non-noble metal catalyst with rich resources, high efficiency and outstanding stability is developed to replace noble metal, and the 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-dopedcarbomatrix, co@N-CNTs@rGO and the like are attracting attention due to their excellent catalytic properties.
There are many methods for preparing the reduced graphene oxide composite metal nano-array catalyst, wherein the most widely used method is a chemical vapor deposition method, cobalt chloride and Metal Organic Frameworks (MOFs) are used as raw materials, and the carbon-based metal catalyst is obtained through high-temperature calcination, but the existing preparation method has long period, the used raw materials are expensive, and the large-scale production cost is high.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of the reduced graphene oxide composite metal nano-array catalyst, which has the advantages of low price of raw materials, simple preparation process, safety, short period, simple required equipment and suitability for mass production.
The invention is realized by the following technical scheme.
The preparation method of the 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 160-200 ℃ to prepare a carbon cloth precursor;
s2, loading soluble cobalt salt on the carbon cloth precursor prepared in the step S1, and carrying out annealing treatment at 300-600 ℃ in a reducing gas atmosphere to prepare the reduced graphene oxide composite metal nano array catalyst.
Preferably, in the step S1, the medium is a mixed solution prepared from water and ethanol according to a volume ratio of 1:1.
Preferably, in S1, the dosage ratio of the graphene oxide to the medium is 0.04 to 0.06g:30ml.
Preferably, in S1, the carbon cloth is sonicated in nitric acid in advance, then sonicated in water, and finally sonicated in ethanol.
Preferably, in S1, the reaction time is from 10 to 15 hours.
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 gas mixture, and the gas flow is kept at 100mL/min.
Preferably, in S2, the temperature is heated from room temperature to 300-600 ℃ at a heating rate of 5 ℃/min, and the temperature is kept for 1-6 hours.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the preparation method, graphene oxide and carbon cloth are subjected to hydrothermal treatment and then are subjected to low-temperature drying to obtain a precursor, the precursor and a cobalt nitrate hexahydrate solution are mixed and subjected to annealing treatment in a reducing gas atmosphere, and the reduced graphene oxide composite metal nano-array catalyst can be prepared through a hydrothermal-chemical vapor deposition two-step method;
2. the catalyst provided by the invention directly grows on the carbon cloth without using a polymer adhesive, so that the conductivity is improved; and the product obtained by the preparation method can obtain the reduced graphene oxide composite metal nano array catalyst without washing, and the operation process is simpler.
Drawings
FIG. 1 is a powder X-ray diffraction pattern of the reduced graphene oxide composite metal nano-array catalyst 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 nano-array catalyst;
FIG. 3 is a graph of oxygen evolution performance of a reduced graphene oxide composite metal nanoarray catalyst.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the present invention will be further described with reference to the specific examples and the accompanying drawings, but the examples are not intended to be limiting.
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 160-200 ℃ to prepare a carbon cloth precursor;
s2, loading soluble cobalt salt on the carbon cloth precursor prepared in the step S1, and carrying out annealing treatment at 300-600 ℃ in a reducing gas atmosphere to prepare the reduced graphene oxide composite metal nano array catalyst.
The method is to compound metal Co and graphene oxide, and the same suitable metals include Fe, ni, cu, bi, W, sn, in, ce and Ga.
Example 1
The preparation method of the 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 polytetrafluoroethylene-lined stainless steel autoclave, performing ultrasonic treatment for 30min to form a suspension, adding the treated carbon cloth (firstly, performing ultrasonic treatment in 3mol/L nitric acid solution for 30min; then performing ultrasonic treatment in deionized water for 30min; finally performing ultrasonic treatment in ethanol for 30 min), and reacting the treated carbon cloth in a 180 ℃ oven for 12h; 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 hydrogen and argon mixed gas for 30min to remove air, and keeping the flow of the hydrogen and argon mixed gas at 100mL/min; heating the tube furnace from room temperature to 450 ℃ at a heating rate of 5 ℃/min, and preserving heat for 4 hours; and (3) after the temperature is naturally reduced to the room temperature, closing the hydrogen-argon mixed gas flow, and taking out the sintered black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 2
The preparation method of the 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 polytetrafluoroethylene-lined stainless steel autoclave, performing ultrasonic treatment for 30min to form a suspension, adding the treated carbon cloth (firstly, performing ultrasonic treatment in 3mol/L nitric acid solution for 30min; then performing ultrasonic treatment in deionized water for 30min; finally performing ultrasonic treatment in ethanol for 30 min), and reacting the treated carbon cloth in a 180 ℃ oven for 12h; 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 hydrogen and argon mixed gas for 30min to remove air, and keeping the flow of the hydrogen and argon mixed gas at 100mL/min; heating the tube furnace from room temperature to 500 ℃ at a heating rate of 5 ℃/min, and preserving heat for 4 hours; and (3) after the temperature is naturally reduced to the room temperature, closing the hydrogen-argon mixed gas flow, and taking out the sintered black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 3
The preparation method of the 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 polytetrafluoroethylene-lined stainless steel autoclave, performing ultrasonic treatment for 30min to form a suspension, adding the treated carbon cloth (firstly, performing ultrasonic treatment in 3mol/L nitric acid solution for 30min; then performing ultrasonic treatment in deionized water for 30min; finally performing ultrasonic treatment in ethanol for 30 min), and reacting the treated carbon cloth in a 180 ℃ oven for 12h; 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 hydrogen and argon mixed gas for 30min to remove air, and keeping the flow of the hydrogen and argon mixed gas at 100mL/min; heating the tube furnace from room temperature to 400 ℃ at a heating rate of 5 ℃/min, and preserving the heat for 4 hours; and (3) after the temperature is naturally reduced to the room temperature, closing the hydrogen-argon mixed gas flow, and taking out the sintered black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 4
The preparation method of the 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 polytetrafluoroethylene-lined stainless steel autoclave, performing ultrasonic treatment for 30min to form a suspension, adding the treated carbon cloth (firstly, performing ultrasonic treatment in 3mol/L nitric acid solution for 30min; then performing ultrasonic treatment in deionized water for 30min; finally performing ultrasonic treatment in ethanol for 30 min), and reacting the treated carbon cloth in a 180 ℃ oven for 12h; washing the obtained carbon cloth precursor with deionized water, and drying in a vacuum drying oven at 60 ℃ for 24 hours;
then, 0.294g of cobalt nitrate hexahydrate is dissolved in 15mL of ethanol, a carbon cloth precursor is added after the cobalt nitrate hexahydrate is fully dissolved, the carbon cloth precursor is heated at 60 ℃ to remove a solvent, after standing for 12 hours, the obtained pink carbon cloth sample and a porcelain boat are put into a quartz tube furnace, hydrogen and argon mixed gas is firstly introduced for 30 minutes to remove air, and the flow of the hydrogen and argon mixed gas is kept at 100mL/min; heating the tube furnace from room temperature to 450 ℃ at a heating rate of 5 ℃/min, and preserving heat for 4 hours; and (3) after the temperature is naturally reduced to the room temperature, closing the hydrogen-argon mixed gas flow, and taking out the sintered black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 5
The preparation method of the 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 polytetrafluoroethylene-lined stainless steel autoclave, performing ultrasonic treatment for 30min to form a suspension, adding the treated carbon cloth (firstly, performing ultrasonic treatment in 3mol/L nitric acid solution for 30min; then performing ultrasonic treatment in deionized water for 30min; finally performing ultrasonic treatment in ethanol for 30 min), and reacting the treated carbon cloth in a 180 ℃ oven for 12h; 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 fully dissolving, 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 hydrogen and argon mixed gas for 30min to remove air, and keeping the flow of the hydrogen and argon mixed gas at 100mL/min; heating the tube furnace from room temperature to 450 ℃ at a heating rate of 5 ℃/min, and preserving heat for 4 hours; and (3) after the temperature is naturally reduced to the room temperature, closing the hydrogen-argon mixed gas flow, and taking out the sintered black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 6
The preparation method of the 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 polytetrafluoroethylene-lined stainless steel autoclave, performing ultrasonic treatment for 30min to form a suspension, adding the treated carbon cloth (firstly, performing ultrasonic treatment in 3mol/L nitric acid solution for 30min; then performing ultrasonic treatment in deionized water for 30min; finally performing ultrasonic treatment in ethanol for 30 min), and reacting the treated carbon cloth in a 180 ℃ oven for 12h; 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 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 a hydrogen-argon mixed gas for 30min to remove air, and keeping the hydrogen-argon mixed gas flow at 100mL/min; heating the tube furnace from room temperature to 450 ℃ at a heating rate of 5 ℃/min, and preserving heat for 4 hours; and (3) after the temperature is naturally reduced to the room temperature, closing the hydrogen-argon mixed gas flow, and taking out the sintered black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 7
The preparation method of the 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 polytetrafluoroethylene-lined stainless steel autoclave, performing ultrasonic treatment for 30min to form a suspension, adding the treated carbon cloth (firstly, performing ultrasonic treatment in 3mol/L nitric acid solution for 30min; then performing ultrasonic treatment in deionized water for 30min; finally performing ultrasonic treatment in ethanol for 30 min), and reacting the treated carbon cloth in a 180 ℃ oven for 12h; 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 hydrogen and argon mixed gas for 30min to remove air, and keeping the flow of the hydrogen and argon mixed gas at 100mL/min; heating the tube furnace from room temperature to 450 ℃ at a heating rate of 5 ℃/min, and preserving heat for 4 hours; and (3) after the temperature is naturally reduced to the room temperature, closing the hydrogen-argon mixed gas flow, and taking out the sintered black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Example 8
The preparation method of the 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 polytetrafluoroethylene-lined stainless steel autoclave, performing ultrasonic treatment for 30min to form a suspension, adding the treated carbon cloth (firstly, performing ultrasonic treatment in 3mol/L nitric acid solution for 30min; then performing ultrasonic treatment in deionized water for 30min; finally performing ultrasonic treatment in ethanol for 30 min), and reacting the treated carbon cloth in a 180 ℃ oven for 12h; 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 hydrogen and argon mixed gas for 30min to remove air, and keeping the flow of the hydrogen and argon mixed gas at 100mL/min; heating the tube furnace from room temperature to 450 ℃ at a heating rate of 5 ℃/min, and preserving heat for 4 hours; and (3) after the temperature is naturally reduced to the room temperature, closing the hydrogen-argon mixed gas flow, and taking out the sintered black solid to obtain the reduced graphene oxide composite metal nano array catalyst.
Since the morphology structure and performance of the reduced graphene oxide composite metal nano-array catalyst prepared in the above embodiment are substantially the same, only the performance of the catalyst prepared in embodiment 1 will be described below. The prepared catalyst was subjected to X-ray diffraction, and the result is shown in FIG. 1. As can be seen from FIG. 1, XRD peak positions appear at 44.8, 47.6 and 75.9 degrees respectively at (002), (101) and (110) planes (PDF#05-0727), 51.5 degrees respectively at (200) planes (PDF#15-0806), and 26.4 and 42.5 degrees respectively at (002) and (100) planes (PDF#41-1487), which indicates that the Co/RGO/CC catalyst is successfully prepared.
The electrochemical performance of the prepared catalyst is tested, and the results are shown in fig. 2 and 3. As can be seen from FIG. 2, co/RGO/CC has a current density of 10mA.cm in an alkaline solution -2 The required hydrogen evolution overpotential is 96mV; as can be seen from FIG. 3, co/RGO/CC has a current density of 10mA.cm in an alkaline solution -2 The required oxygen evolution overpotential was 301mV; illustrating the catalyst prepared by the inventionThe catalyst has better catalytic performance.
It should be noted that, when reference is made to a numerical range in the claims of the present invention, it should be understood that two endpoints of each numerical range and any numerical value between the two endpoints are optional, and since the adopted steps are the same as those of the embodiments, the present invention describes the preferred embodiments, but once the basic inventive concepts are known to those skilled in the art, additional variations and modifications may be made to the embodiments. It is therefore intended that the following claims be interpreted as including the 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 modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that such modifications and variations be included herein within the scope of the appended claims and their equivalents.
Claims (7)
1. The preparation method of the reduced graphene oxide composite metal nano-array catalyst is characterized by comprising the following steps of:
s1, dispersing graphene oxide in a medium to prepare a suspension, adding carbon cloth, and reacting at 160-200 ℃ to prepare a carbon cloth precursor; the medium is a mixed solution prepared from water and ethanol according to a volume ratio of 1:1; the dosage ratio of the graphene oxide to the medium is 0.04-0.06 g:30ml;
s2, loading soluble cobalt salt on the carbon cloth precursor prepared in the step S1, and carrying out annealing treatment at 300-600 ℃ in a reducing gas atmosphere to prepare the reduced graphene oxide composite metal nano array catalyst.
2. The method for preparing a reduced graphene oxide composite metal nano-array catalyst according to claim 1, wherein in S1, the carbon cloth is subjected to ultrasonic treatment in nitric acid in advance, then subjected to ultrasonic treatment in water, and finally subjected to ultrasonic treatment in ethanol.
3. The method for preparing the reduced graphene oxide composite metal nano-array catalyst according to claim 1, wherein in the step S1, the reaction time is 10-15h.
4. The method for preparing the reduced graphene oxide composite metal nano-array catalyst according to claim 1, wherein in the step S2, a soluble cobalt salt is firstly dissolved in ethanol, then an 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 the step S1.
5. The method for preparing a reduced graphene oxide composite metal nano-array catalyst according to claim 1, wherein in S2, the soluble cobalt salt is cobalt nitrate hexahydrate.
6. The method for preparing the reduced graphene oxide composite metal nano-array catalyst according to claim 1, wherein in S2, the reducing gas is a hydrogen-argon gas mixture, and the gas flow is kept at 100mL/min.
7. The method for preparing the reduced graphene oxide composite metal nano-array catalyst according to claim 1, wherein in S2, the temperature is heated from room temperature to 300-600 ℃ at a heating rate of 5 ℃/min, and the temperature is kept for 1-6h.
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