CN114574890B - Self-forming phosphorus-doped redox graphene aerogel catalyst and preparation method and application thereof - Google Patents
Self-forming phosphorus-doped redox graphene aerogel catalyst and preparation method and application thereof Download PDFInfo
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- CN114574890B CN114574890B CN202210273645.7A CN202210273645A CN114574890B CN 114574890 B CN114574890 B CN 114574890B CN 202210273645 A CN202210273645 A CN 202210273645A CN 114574890 B CN114574890 B CN 114574890B
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Abstract
The invention is thatThe invention relates to the technical field of biochemistry, in particular to a self-forming phosphorus-doped redox graphene aerogel catalyst and a preparation method and application thereof. According to the invention, the self-forming phosphorus doped redox graphene aerogel catalyst is prepared by in-situ doping of phosphorus atoms on graphene, and is used as a self-supporting catalyst, so that CO is efficiently and stably realized under low potential 2 Reducing to ethanol.
Description
Technical Field
The invention relates to the technical field of biochemistry, in particular to a self-forming phosphorus-doped redox graphene aerogel catalyst and a preparation method and application thereof.
Background
With the rapid development of economy and the massive combustion of fossil fuels, the carbon dioxide gas emitted by human beings to the atmosphere is rapidly increased, and the energy shortage and the greenhouse effect caused by the rapid increase are also aggravated, so that the living environment and ecological balance of human beings are seriously influenced. CO 2 As an economical, safe, sustainable carbon-oxygen resource compound, the potential for conversion to chemicals or fuels is enormous; the renewable energy source is utilized to drive CO at normal temperature and normal pressure 2 Electrochemical reduction into carbon-containing chemicals or fuels not only can realize cyclic utilization of carbon resources, but also can effectively reduce CO in the atmosphere 2 One of the methods of concentration. Due to CO 2 Stable chemical property and can utilize CO in actual industrial process 2 Is not very reactive, e.g. carbonate synthesis, methanol synthesis, CO of methane 2 Reforming, etc., which are all required to be carried out under severe conditions such as high temperature, high pressure, etc., are high-energy-consumption and low-efficiency processes.
In CO 2 Among the numerous products of reduction, C1 chemicals (such as CO and formic acid) are most common, and multi-carbon chemicals such as ethanol, which have a high energy density (26.8 MJ kg -1 ) And the product easy to store has more research value. Generally only copper-based catalysts will convert CO 2 Reduction ofEthanol, but the reaction process involves multi-step proton-electron transfer and C-C coupling processes, so that the variety of products is more, and the selectivity of ethanol is poor; in addition CO on copper-based catalyst 2 The reaction to ethanol needs to be driven by a higher overpotential (greater than 1V), so that the energy utilization efficiency is low and the stability is poor.
The nonmetallic carbon material has the advantages of wide sources, easy modification, good thermal and mechanical stability and the like, has great application prospect in the aspect of electrochemical reaction, but the pure carbon material is directly applied to the electrochemical reaction due to uniform surface charge distribution and symmetrical spin, so that the effect is not ideal; the electrochemical performance of carbon materials can be generally improved by introducing hetero atoms (such as nitrogen, sulfur, phosphorus, boron, etc.), because hetero atoms with different atomic radii and electronegativity can adjust the spin density or charge distribution of the carbon atoms, thereby changing the surface electron structure of the carbon material to form CO 2 Reduced active sites. Nitrogen doped carbon materials are currently most studied because nitrogen atoms have a higher electronegativity than carbon atoms and can activate CO by delocalizing pi-orbital electrons to break the electroneutrality of the carbon material 2 A molecule; however, the experimental results show that the nitrogen-doped carbon catalyst reduces CO 2 The product is CO and the current density is low<2mA cm -2 ) In addition, the high spin density of nitrogen atoms is also beneficial to the occurrence of competing reactions of hydrogen evolution of electrolyzed water.
The phosphorus atoms have the same valence number as the nitrogen atoms, but have lower electronegativity and larger atomic radius. However, according to literature reports, phosphorus doped nonmetallic catalysts are used for CO 2 The poor reduction activity may be due to the microstructure of the catalyst and the low phosphorus loading.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a self-forming phosphorus-doped redox graphene aerogel catalyst, and a preparation method and application thereof, wherein the self-forming phosphorus-doped redox graphene aerogel catalyst is prepared by in-situ doping of phosphorus atoms on graphene, and is used as a self-supporting catalyst, so that the self-forming phosphorus-doped redox graphene aerogel catalyst is efficient and stable under low potentialCO is now reacted with 2 Reducing to ethanol.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a self-forming phosphorus-doped redox graphene aerogel catalyst comprises the following steps of;
(1) Dispersing graphene oxide in deionized water to obtain graphene oxide dispersion liquid;
(2) Adding phosphoric acid into the graphene oxide dispersion liquid in the step (1), uniformly mixing, performing hydrothermal reaction at 150-180 ℃ for 6-20 hours, and cooling to room temperature to obtain phosphorus doped graphene oxide hydrogel;
(3) And (3) washing and freeze-drying the phosphorus-doped graphene oxide hydrogel obtained in the step (2), calcining for 30-120min at 800-1000 ℃ under the protection of nitrogen, and cooling to room temperature to obtain the self-formed phosphorus-doped redox graphene aerogel catalyst.
Preferably, the graphene oxide in the step (1) is prepared by adopting a modified Hummer method, and the concentration of the graphene oxide dispersion liquid is 0.5-5 mg/mL.
Preferably, the volume ratio of the phosphoric acid to the graphene oxide aqueous solution in the step (2) is 1-5:30.
Preferably, the mixing method in the step (2) adopts ultrasonic dispersion, and the ultrasonic conditions are as follows: ultrasonic treatment is carried out for 30-90 min under 2000-4000 Hz.
Preferably, the washing method in the step (3) adopts water/ethanol alternate soaking washing.
Preferably, the step (3) is freeze-dried to constant weight under the condition that the freeze-drying is carried out for 24-72 hours at the temperature of minus 20-minus 40 ℃.
The invention also protects the self-forming phosphorus-doped redox graphene aerogel catalyst prepared by the preparation method.
The invention also protects the application of the self-formed phosphorus-doped redox graphene aerogel catalyst in preparing an electrochemical catalyst, wherein the electrochemical catalyst is a catalyst for preparing ethanol by electrochemically reducing carbon dioxide.
Compared with the prior art, the invention has the beneficial effects that:
1. the self-forming phosphorus-doped redox graphene aerogel catalyst prepared by the invention can be directly used as a self-supporting working electrode, and can be used as an electrode through direct aerogel compaction so as to carry out CO (carbon monoxide) 2 And the reduction reaction test avoids the complicated working electrode manufacturing steps.
2. According to the invention, firstly, a self-forming phosphorus-doped graphene oxide hydrogel is prepared through a hydrothermal self-assembly method, and then, the phosphorus-doped graphene aerogel catalyst is obtained through high-temperature calcination. The phosphorus-doped graphene aerogel prepared by the method can increase the phosphorus content to 2.71at%, the three-dimensional porous structure of the graphene aerogel is beneficial to electron transmission and electrolyte diffusion, and the high specific surface can be CO 2 Reduction provides a rich active site; the catalyst can convert CO 2 High-efficiency reduction to ethanol, high current density and high ethanol yield, and not only changes the problem that the traditional nitrogen doped nonmetallic catalyst can not convert CO 2 The reduction to a multi-carbon liquid phase product has the disadvantages that the ethanol yield is far higher than the values obtained on other nonmetallic catalysts, and is CO 2 The new method is provided for preparing the ethanol by reduction.
3. The self-forming phosphorus-doped redox graphene aerogel catalyst prepared by the invention can convert CO 2 The catalyst is stably and efficiently reduced into ethanol, and has higher current density and long-cycle stability compared with the nitrogen-doped nonmetallic carbon material catalyst reported in the prior art, and the yield of the obtained ethanol is far higher than the value reported in the prior art; and the carbon material has wide sources and good stability, and the self-formed phosphorus-doped redox graphene aerogel catalyst prepared by the invention is expected to replace the traditional copper-based catalyst to produce ethanol.
Drawings
FIG. 1 is a flow chart of the preparation of the self-forming phosphorus-doped redox graphene aerogel catalyst of examples 1-3 of the present invention;
FIG. 2 is a SEM (a) and TEM (b) images of PGA-1 prepared according to example 1 of the present invention;
FIG. 3 is a SEM (a) and TEM (b) images of PGA-2 prepared according to example 2 of the present invention;
FIG. 4 is a SEM (a) and TEM (b) images of PGA-3 prepared according to example 3 of the present invention;
FIG. 5 shows XRD patterns of catalysts prepared in examples 1, 2 and 3 according to the present invention;
FIG. 6 shows the adsorption-desorption isotherms of nitrogen of the catalysts prepared in examples 1, 2 and 3 of the present invention;
FIG. 7 is a high resolution XPS plot of the catalyst P2P prepared in examples 1, 2, and 3 of the present invention;
FIG. 8 shows the CO at different potentials of PGA-1 prepared in example 1 of the present invention 2 A reduced product faraday efficiency profile;
FIG. 9 shows the CO at different potentials of PGA-2 prepared in example 2 of the present invention 2 A reduced product faraday efficiency profile;
FIG. 10 shows the CO at different potentials of PGA-1 prepared in example 3 of the present invention 2 A reduced product faraday efficiency profile;
FIG. 11 is a graph showing ethanol yields at different potentials for the catalysts prepared in examples 1, 2, and 3 of the present invention;
FIG. 12 shows the PGA-1 at-0.8V prepared in example 1 of the present invention RHE Lower CO 2 And (5) reducing a stability test result graph.
Detailed Description
The following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The experimental methods described in the examples of the present invention are conventional methods unless otherwise specified.
Example 1
A preparation method of a self-forming phosphorus-doped redox graphene aerogel catalyst comprises the following steps:
(1) Preparing Graphene Oxide (GO) by adopting an improved Hummer method, and dispersing the graphene oxide in deionized water to obtain graphene oxide dispersion liquid (GO dispersion liquid);
(2) 1mL of phosphoric acid was placed in 2mg mL -1 、30In the mL GO dispersion liquid, ultrasonically dispersing the mixed liquid for 1h, transferring the mixed liquid into a 50mL polytetrafluoroethylene lining reaction kettle, reacting for 12h at 180 ℃, and cooling the reaction kettle to room temperature to obtain phosphorus doped graphene oxide hydrogel;
(3) Taking out the phosphorus doped graphene oxide hydrogel, soaking and washing with water/ethanol, then placing in a freeze dryer for freeze-drying for 48 hours, placing the freeze-dried sample in a tube furnace, calcining for 1 hour at 900 ℃ under the protection of nitrogen, cooling to room temperature, taking out, and obtaining the self-formed phosphorus doped redox graphene aerogel catalyst, which is marked as PGA-1.
Example 2
A preparation method of a self-forming phosphorus-doped redox graphene aerogel catalyst comprises the following steps:
(1) Preparing Graphene Oxide (GO) by adopting an improved Hummer method, and dispersing the graphene oxide in deionized water to obtain graphene oxide dispersion liquid (GO dispersion liquid);
(2) 2mL of phosphoric acid was taken and placed in 2mg mL -1 In 30mL of GO dispersion liquid, ultrasonically dispersing the mixed liquid for 1h, transferring the mixed liquid into a 50mL polytetrafluoroethylene lining reaction kettle, reacting for 12h at 180 ℃, and cooling the reaction kettle to room temperature to obtain phosphorus doped graphene oxide hydrogel;
(3) Taking out the phosphorus doped graphene oxide hydrogel, soaking and washing with water/ethanol, then placing in a freeze dryer for freeze-drying for 48 hours, placing the freeze-dried sample in a tube furnace, calcining for 1 hour at 900 ℃ under the protection of nitrogen, cooling to room temperature, taking out, and obtaining the self-formed phosphorus doped graphene aerogel catalyst, which is marked as PGA-2.
Example 3
A preparation method of a self-forming phosphorus-doped redox graphene aerogel catalyst comprises the following steps:
(1) Preparing Graphene Oxide (GO) by adopting an improved Hummer method, and dispersing the graphene oxide in deionized water to obtain graphene oxide dispersion liquid (GO dispersion liquid);
(2) 3mL of phosphoric acid was taken and placed in 2mg mL -1 In 30mL of GO dispersion liquid, the mixed liquid is dispersed for 1h by ultrasonic, and thenTransferring the mixture into a 50mL polytetrafluoroethylene lining reaction kettle, reacting for 12 hours at 180 ℃, and cooling the reaction kettle to room temperature to obtain phosphorus doped graphene oxide hydrogel;
(3) Taking out the graphene hydrogel obtained by doping the graphene oxide hydrogel with phosphorus, soaking and washing with water/ethanol, then placing in a freeze dryer for freeze-drying for 48 hours, placing the freeze-dried sample in a tube furnace, calcining for 1 hour at 900 ℃ under the protection of nitrogen, cooling to room temperature, taking out, and obtaining the self-formed phosphorus-doped graphene aerogel catalyst, which is marked as PGA-3.
Example 4
A preparation method of a self-forming phosphorus-doped redox graphene aerogel catalyst comprises the following steps:
(1) Preparing Graphene Oxide (GO) by adopting an improved Hummer method, and dispersing the graphene oxide in deionized water to obtain graphene oxide dispersion liquid (GO dispersion liquid);
(2) 3mL of phosphoric acid was placed in 0.5mg mL -1 In 30mL of GO dispersion liquid, ultrasonically dispersing the mixed liquid for 90min, transferring the mixed liquid into a 50mL polytetrafluoroethylene lining reaction kettle, reacting for 6h at 170 ℃, and cooling the reaction kettle to room temperature to obtain phosphorus doped graphene oxide hydrogel;
(3) Taking out the graphene hydrogel obtained by doping the graphene oxide hydrogel with phosphorus, soaking and washing with water/ethanol, then placing in a freeze dryer for freeze-drying for 48 hours, placing the freeze-dried sample in a tube furnace, calcining for 120 minutes at 800 ℃ under the protection of nitrogen, cooling to room temperature, and taking out to obtain the self-formed phosphorus-doped graphene aerogel catalyst.
Example 5
A preparation method of a self-forming phosphorus-doped redox graphene aerogel catalyst comprises the following steps:
(1) Preparing Graphene Oxide (GO) by adopting an improved Hummer method, and dispersing the graphene oxide in deionized water to obtain graphene oxide dispersion liquid (GO dispersion liquid);
(2) 3mL of phosphoric acid was placed in 5mg mL -1 In 30mL of GO dispersion, the mixed solution is dispersed for 30min by ultrasonic, and then is transferred to 50mL of polymerReacting for 20 hours at 150 ℃ in a tetrafluoroethylene lining reaction kettle, and cooling the reaction kettle to room temperature to obtain phosphorus doped graphene oxide hydrogel;
(3) Taking out the graphene hydrogel obtained by doping the graphene oxide hydrogel with phosphorus, soaking and washing with water/ethanol, then placing in a freeze dryer for freeze-drying for 48 hours, placing the freeze-dried sample in a tube furnace, calcining for 30 minutes at 1000 ℃ under the protection of nitrogen, cooling to room temperature, and taking out to obtain the self-formed phosphorus-doped graphene aerogel catalyst.
Examples 1 to 5 of the invention all produce CO 2 The self-forming phosphorus-doped redox graphene aerogel catalyst stably and efficiently reduced to ethanol is exemplified by the products of examples 1-3, and the self-forming phosphorus-doped redox graphene aerogel catalyst prepared in examples 1-3 is subjected to performance study, and the specific study method and results are as follows:
CO 2 method of reduction reaction test:
the three-electrode H-type electrolytic tank is adopted, the prepared phosphorus doped graphene aerogel is used as a working electrode in a cathode tank, ag/AgCl is used as a reference electrode, a graphite rod is used as a counter electrode in an anode tank, and 0.5mol/L KHCO is used 3 The solution is an electrolyte.
Study results:
the results of fig. 2, 3 and 4 show that the obtained catalyst is a three-dimensional porous structure assembled by layered graphene.
The results in FIG. 5 show that the broad peaks at 24.5℃and 43.3℃correspond to the (002) and (100) planes of amorphous carbon, respectively, and that the catalyst is composed of amorphous carbon and contains no metal element.
The results of fig. 6 demonstrate that the self-forming phosphorus-doped redox graphene aerogel catalysts prepared in examples 1-3 all exhibit type IV adsorption isotherms, illustrating that the samples prepared in examples 1-3 are each composed of micro-mesoporous, hierarchical pores.
The results of fig. 7 show that the self-forming phosphorus-doped redox graphene aerogel catalysts prepared in examples 1-3 are located at 132.3 and 133.9eV, and feature peaks are generated, which correspond to P-C bonds and P-O bonds respectively, and the P element content of the catalysts obtained in examples 1, 2 and 3 measured by XPS is shown in table 1, which indicates that phosphorus doping is realized in graphene in the application.
Table 1 XPS table of the P element content of the catalysts obtained in examples 1, 2, 3
| Examples | 1 | 2 | 3 |
| P element content (at%) | 1.78 | 2.31 | 2.71 |
FIG. 8 shows the results of PGA-1 versus CO using the catalyst prepared in example 1 2 Reduction is carried out, and the gas product is H 2 And CO, with very little CO production, ethanol being the only liquid product, with the highest Faraday efficiency at-0.9V, up to 34.3%.
FIG. 9 shows the results of PGA-2 versus CO using the catalyst prepared in example 2 2 Reduction is carried out, and the gas product is H 2 And CO, with very little CO production, ethanol being the only liquid product, with the highest Faraday efficiency at-0.8V, up to 48.7%.
FIG. 10 shows the result of PGA-3 vs. CO using the catalyst prepared in example 3 2 Reduction is carried out, and the gas product is H 2 And CO, with very little CO production, ethanol being the only liquid product, with the highest Faraday efficiency at-0.8V, up to 40.7%.
The results of FIG. 11 show thatThe PGA-2 obtained in example 2 showed the best catalytic effect at various voltages, compared with example 1 and example 3, and the ethanol yield at-0.9V was the highest, and was 15.7. Mu. Mol h -1 cm -2 。
FIG. 12 shows that PGA-1 prepared in example 1 was at-0.8V RHE Lower CO 2 As a result of the reduction stability test, the catalyst can stably work for 70 hours and has excellent long-time stability.
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 the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof. The above-described embodiments are merely preferred embodiments for fully explaining the present invention, and the scope of protection is not limited thereto.
Claims (7)
1. The preparation method of the self-forming phosphorus-doped redox graphene aerogel catalyst is characterized by comprising the following steps of;
(1) Dispersing graphene oxide in deionized water to obtain graphene oxide dispersion liquid;
(2) Adding phosphoric acid into the graphene oxide dispersion liquid in the step (1), uniformly mixing, performing hydrothermal reaction at 150-180 ℃ for 6-20 hours, and cooling to room temperature to obtain phosphorus doped graphene oxide hydrogel;
(3) Washing and freeze-drying the phosphorus-doped graphene oxide hydrogel obtained in the step (2), calcining for 30-120min at 800-1000 ℃ under the protection of nitrogen, and cooling to room temperature to obtain the self-formed phosphorus-doped redox graphene aerogel catalyst;
the volume ratio of the phosphoric acid to the graphene oxide aqueous solution in the step (2) is 1-5:30.
2. The method for preparing the self-forming phosphorus-doped redox graphene aerogel catalyst according to claim 1, wherein the graphene oxide obtained in the step (1) is prepared by adopting a modified Hummer method, and the concentration of the graphene oxide dispersion liquid is 0.5-5 mg/mL.
3. The method for preparing the self-forming phosphorus-doped redox graphene aerogel catalyst according to claim 1, wherein the mixing method in the step (2) adopts ultrasonic dispersion, and the ultrasonic conditions are as follows: ultrasonic treatment is carried out for 30-90 min under 2000-4000 Hz.
4. The method for preparing the self-forming phosphorus-doped redox graphene aerogel catalyst according to claim 1, wherein the washing method in the step (3) adopts water/ethanol alternate impregnation washing.
5. The method for preparing the self-forming phosphorus-doped redox graphene aerogel catalyst according to claim 1, wherein the step (3) is performed by freeze-drying to constant weight under the condition of freeze-drying at-20 to-40 ℃ for 24-72 h.
6. A self-forming phosphorus-doped redox graphene aerogel catalyst made by the method of any of claims 1-5.
7. Use of the self-forming phosphorus-doped redox graphene aerogel catalyst of claim 6 in the preparation of an electrochemical catalyst, wherein the electrochemical catalyst is a catalyst for electrochemical reduction of carbon dioxide to ethanol.
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