CN114649538B - Electro-catalyst for preparing hydrogen by methanol electrolysis and preparation method thereof - Google Patents
Electro-catalyst for preparing hydrogen by methanol electrolysis and preparation method thereof Download PDFInfo
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- CN114649538B CN114649538B CN202210300797.1A CN202210300797A CN114649538B CN 114649538 B CN114649538 B CN 114649538B CN 202210300797 A CN202210300797 A CN 202210300797A CN 114649538 B CN114649538 B CN 114649538B
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
The invention discloses an electro-catalyst for preparing hydrogen by methanol electrolysis, which takes molybdenum telluride doped with nitrogen and phosphorus as a composite carrier and platinum-based nano particles as a carrier, and the formed catalyst can be used for acidic methanol electrolysis reaction; the aggregation of the platinum-based noble metal nano particles is inhibited through the interaction between the metal and the carrier, so that the utilization rate of the platinum-based noble metal is improved; the oxygen-philic characteristic of molybdenum telluride can weaken the adsorption energy of a carbon monoxide-like intermediate in the anodic methanol oxidation process, and reduce the carbon monoxide poisoning capacity in the methanol oxidation reaction; the nitrogen-phosphorus doping effect can adjust the electronic structure of the platinum-based noble metal, optimize the electron transmission of the active site and the gibbs free energy of hydrogen adsorption, and is beneficial to improving the efficiency of the cathodic hydrogen evolution reaction; the electrocatalyst obtained by the invention has higher electrocatalytic activity and stability, and has wide application prospect in the field of hydrogen production by methanol electrolysis.
Description
Technical Field
The invention relates to an electro-catalyst for producing hydrogen by methanol electrolysis, and also relates to a preparation method of the electro-catalyst for producing hydrogen by methanol electrolysis.
Background
With the rapid increase in global environmental problems caused by fossil energy consumption, searching for sustainable green energy has become an urgent need. Hydrogen is attracting attention as a promising clean, renewable energy source. Currently, hydrogen is mainly derived from steam reforming of fossil fuels (methane or coal) and electrocatalytic hydrocracking in industrial production. However, the kinetics of the oxygen evolution reaction of electrolyzed water on the anode is slow, and the oxidation potential of methanol is much lower than that of water compared with electrolyzed water, indicating that the use of methanol oxidation as the anode reaction can significantly reduce the consumption of electrical energy. At present, platinum-based catalysts are still the most widely used catalysts for methanol oxidation and hydrogen evolution reactions. However, due to the high price of precious metals and limited resources, the use of Pt-based catalysts to increase the catalytic activity of methanol oxidation and hydrogen evolution reactions is not a long-term viable solution. In addition, the carbon monoxide-like carbonaceous intermediate generated in the methanol oxidation process has strong adsorption and catalytic inhibition effects on methanol, and easily pollutes the active site of Pt. In the prior art, alloying platinum with transition metal elements is the most common method for improving the catalytic activity of methanol oxidation reaction and hydrogen evolution reaction. The catalytic performance of the platinum-based catalyst is enhanced by an electronic effect, a strain effect, or a synergistic effect. However, the acidic electrolyte has the problems of easy dissolution of alloy, strong adsorption of carbon monoxide and carbonaceous intermediates on the surface of noble metal, and the like, and the prepared catalyst has poor electrocatalytic performance.
Disclosure of Invention
The invention aims to: aiming at the problem of low electrocatalytic performance of a catalyst for producing hydrogen by methanol electrolysis in the prior art, the invention provides a catalyst for producing hydrogen by methanol electrolysis, which is prepared by loading molybdenum telluride doped with carbon and nitrogen and phosphorus with platinum-based nano particles; also provides a preparation method of the electrocatalyst.
The technical scheme is as follows: the catalyst takes nitrogen-phosphorus doped carbon molybdenum telluride as a composite carrier, and the carrier is platinum-based nano particles.
Preferably, the loading of the platinum-based nano particles is 20-60% of the mass of the whole catalyst.
Preferably, the platinum-based nano particles comprise platinum simple substances or alloys formed by platinum and transition metals; wherein the transition metal comprises palladium, ruthenium, rhodium, silver, gold, cobalt or nickel.
Preferably, the particle size of the platinum-based nanoparticles is 1-10 nm.
The preparation method of the electro-catalyst for preparing hydrogen by methanol electrolysis comprises the following steps:
(1) Dispersing molybdenum trioxide and imidazole in water, refluxing, naturally cooling to room temperature after refluxing, carrying out suction filtration, washing and vacuum drying to obtain Mo-MOF; uniformly mixing the prepared Mo-MOF and tellurium powder, and performing heat treatment under hydrogen-argon mixed gas to obtain nitrogen-doped carbon molybdenum telluride;
(2) Performing heat treatment on the molybdenum telluride doped with carbon by nitrogen and sodium hypophosphite in the step (1) under nitrogen to obtain molybdenum telluride doped with carbon by nitrogen and phosphorus;
(3) Adding the molybdenum telluride doped with carbon by nitrogen and phosphorus and the chloroplatinic acid aqueous solution in the step (2) into ethylene glycol, uniformly stirring, reducing platinum ions into a platinum simple substance by utilizing a microwave-assisted ethylene glycol reduction method, and after the reaction is finished, carrying out suction filtration, washing and vacuum drying to obtain the electrocatalyst of the molybdenum telluride loaded with carbon by nitrogen and phosphorus and platinum-based nano particles.
Preferably, in the step (1), the mass ratio of the molybdenum trioxide to the imidazole is 1-3:1, the reflux temperature is 100-130 ℃, and the reflux time is 10-20 hours.
Preferably, in the step (1), the mass ratio of Mo-MOF to tellurium powder is 1:0.5-2, the heating rate is 2-10 ℃/min under the condition of hydrogen-argon mixed gas, the heat treatment temperature is 800-1000 ℃, the heat treatment time is 1-3 hours, and the volume percentage of hydrogen in the hydrogen-argon mixed gas is 5-10%.
Preferably, in the step (2), the mass ratio of the molybdenum telluride doped with carbon to the sodium hypophosphite is 1:3-8, the heating rate is 2-10 ℃/min under nitrogen, the heat treatment temperature is 150-350 ℃, and the heat treatment time is 1-3 hours.
Preferably, in the step (3), the microwave power is 500-800W, and the microwave time is 2-5 minutes.
According to the invention, the molybdenum telluride doped with carbon and nitrogen is synthesized as a composite carrier, and the platinum-based nano particles are loaded to prepare the methanol electrolysis hydrogen production electrocatalyst, on one hand, electron transfer exists between the platinum-based nano particles and the molybdenum telluride carrier, so that interaction (interaction force enhancement) is generated between the platinum-based nano particles and the carrier, the anchoring capability between the platinum-based nano particles and the carrier is enhanced, and the agglomeration (dispersibility) of the platinum-based nano particles can be inhibited, thereby improving the utilization rate of noble metals. On the other hand, the oxygen-philic characteristic of molybdenum telluride can effectively adjust the position of the center of the platinum-based catalyst d, weaken the adsorption energy of an intermediate (CO), promote the oxidation and removal of the intermediate, and further improve the poisoning resistance (carbon monoxide-like intermediate poisoning resistance) of the catalyst, and further effectively improve the stability of the catalyst. The nitrogen and phosphorus doping can regulate the electronic structure of platinum, so as to optimize the electron transmission of active sites and the free energy of hydrogen adsorption gibbs, thereby being beneficial to improving the efficiency of cathodic hydrogen evolution reaction and improving the electrocatalytic activity of the platinum-based catalyst.
The beneficial effects are that: according to the invention, the platinum-based nano particles in the electrocatalyst are uniformly loaded on the nitrogen-phosphorus doped carbon molybdenum telluride, so that the utilization rate of noble metal platinum can be improved, the poisoning resistance of a carbon monoxide-like intermediate of the platinum-based catalyst can be improved, the stability of the platinum-based catalyst is further improved, and more active sites can be provided by doping nitrogen and phosphorus, so that the catalytic activity of the platinum-based catalyst is effectively improved.
Drawings
FIG. 1 is an XRD pattern of nitrogen-phosphorus doped carbon molybdenum telluride prepared in example 1;
FIG. 2 is an XRD pattern of nitrogen-phosphorus doped carbon molybdenum telluride supported platinum nanoparticles prepared in example 1;
FIG. 3 is a cyclic voltammogram (a) and chronoamperometric test curve (b) for the nitrogen-phosphorus doped carbon molybdenum telluride supported platinum nanoparticle catalyst, the nitrogen doped carbon molybdenum telluride supported platinum nanoparticle catalyst and the commercial Pt/C catalyst in a 0.5mol/L sulfuric acid and 1mol/L methanol mixed solution of example 1;
FIG. 4 is a linear sweep voltammogram (a) and chronoamperometric test curve (b) for the nitrogen-phosphorus doped carbon molybdenum telluride supported platinum nanoparticle catalyst of example 1, a nitrogen doped carbon molybdenum telluride supported platinum nanoparticle catalyst and a commercial Pt/C catalyst in a 0.5mol/L sulfuric acid and 1mol/L methanol mixed solution;
fig. 5 is a linear sweep voltammogram (a) and chronoamperometric test curve (b) for a nitrogen-phosphorus doped carbon molybdenum telluride supported platinum nanoparticle catalyst and a commercial Pt/C catalyst in methanol electrolysis in example 1.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings.
Example 1
a. Preparation of carbon-doped molybdenum telluride
(1) 1.4g of molybdenum trioxide and 0.664g of imidazole were dispersed in 150mL of water and refluxed at 110℃for 12 hours;
(2) Cooling to room temperature, suction filtering, washing with deionized water for at least 3 times, and vacuum drying at 60deg.C overnight;
(3) Uniformly mixing the obtained Mo-MOF and tellurium powder according to the mass ratio of 1:1, and performing heat treatment for 2 hours under the condition of hydrogen-argon mixed gas, wherein the heating rate is 5 ℃/min, the heat treatment temperature is 800 ℃, and the obtained product is named Mo 6 Te 8 N-C; in the hydrogen-argon mixed gas, the volume percentage of hydrogen is 5%;
(4) Adding the obtained molybdenum telluride doped with carbon and sodium hypophosphite into two ends of a porcelain boat respectively according to the mass ratio of 1:5, and performing heat treatment for 2 hours under nitrogen, wherein the heating rate is 5 ℃/min, the heat treatment temperature is 300 ℃, and the obtained product is named Mo 6 Te 8 /N,P-C。
The XRD of the prepared nitrogen-phosphorus doped carbon molybdenum telluride is shown in figure 1, and figure 1 illustrates that the nitrogen-phosphorus doped carbon molybdenum telluride is successfully prepared.
b. Preparation of platinum nanoparticle-loaded nitrogen-phosphorus doped carbon molybdenum telluride
(1) 80mg of prepared Mo 6 Te 8 N, P-C was dispersed in 50mL of ethylene glycol, followed by addition of 670. Mu.L of an aqueous solution of chloroplatinic acid (the content of platinum in the aqueous solution of chloroplatinic acid was 30 mg/mL);
(2) Magnetically stirring to form a uniform suspension, placing the uniform suspension into a microwave reactor, carrying out microwave power of 700W and microwave time of 5 minutes, and naturally cooling to room temperature after reaction;
(3) Suction filtration, washing with ethanol and deionized water for at least 3 times, vacuum drying at 60deg.C overnight, and obtaining product named PtMo 6 Te 8 /N,P-C。
XRD of the resulting nitrogen-phosphorus doped carbon molybdenum telluride loaded with platinum nanoparticles is shown in FIG. 2. As can be seen from fig. 2, the diffraction peaks of Pt correspond to the standard PDF card of platinum, indicating that the successful preparation of the nitrogen-phosphorus doped carbon molybdenum telluride loaded with platinum nanoparticles was achieved.
Example 2
PtMo 6 Te 8 The preparation method of the N-C comprises the following steps:
(1) 1.4g of molybdenum trioxide and 0.664g of imidazole were dispersed in 150mL of water and refluxed at 110℃for 12 hours;
(2) Cooling to room temperature, suction filtering, washing with deionized water for at least 3 times, and vacuum drying at 60deg.C overnight;
(3) Uniformly mixing the obtained Mo-MOF and tellurium powder according to the mass ratio of 1:1, and performing heat treatment for 2 hours under the condition of hydrogen-argon mixed gas, wherein the heating rate is 5 ℃/min, the heat treatment temperature is 800 ℃, and the obtained product is named Mo 6 Te 8 N-C; in the hydrogen-argon mixed gas, the volume percentage of hydrogen is 5%;
(4) 80mg of prepared Mo 6 Te 8 N-C was dispersed in 50mL of ethylene glycol, followed by addition of 670. Mu.L of an aqueous solution of chloroplatinic acid (the content of platinum in the aqueous solution of chloroplatinic acid was 30 mg/mL);
(5) Magnetically stirring to form a uniform suspension, placing the uniform suspension into a microwave reactor, carrying out microwave power of 700W and microwave time of 5 minutes, and naturally cooling to room temperature after reaction;
(6) Suction filtration, washing with ethanol and deionized water for at least 3 times, vacuum drying at 60deg.C overnight, and obtaining product named PtMo 6 Te 8 /N-C。
Example 3
PtMo obtained in example 1 was tested separately 6 Te 8 N, P-C, ptMo obtained in example 2 6 Te 8 Use of/N-C and commercial Pt/C catalysts for catalyzing the oxidation of methanol in an acidic electrolyte:
5mg of PtMo obtained in example 1 was taken 6 Te 8 N, P-C,5mg of PtMo obtained in example 2 6 Te 8 Respectively testing/N-C and 5mg commercial Pt/C catalyst, respectively adding three different catalysts into 950 mu L of anhydrous ethanol and 50 mu L of Nafion mixed solution, and uniformly dispersing by ultrasonic to obtain mixed solution; and (3) dropwise adding 10 mu L of the mixed solution onto the surface of a glassy carbon electrode to serve as a working electrode, a carbon rod to serve as a counter electrode and a Saturated Calomel Electrode (SCE) to serve as a reference electrode, placing the electrode into a sulfuric acid mixed system containing 1mol/L of methanol and 0.5mol/L of sulfuric acid, performing cyclic voltammetry scanning between-0.2V and 1V at a scanning speed of 50mV/s, and performing constant current timing test for 2 hours at a potential of 0.6V.
FIG. 3 shows PtMo 6 Te 8 /N,P-C、PtMo 6 Te 8 Cyclic voltammograms and chronoamperometric test curves of N-C and commercial Pt/C catalysts in a 0.5mol/L sulfuric acid and 1mol/L methanol mixed solution. As can be seen from FIG. 3a, ptMo 6 Te 8 The peak current density value of N, P-C is highest; as can be seen from FIG. 3b, ptMo after 7200s of stability test 6 Te 8 The final current density value of/N, P-C retention is highest. Compared with PtMo 6 Te 8 N-C and commercial Pt/C catalysts, ptMo of this invention 6 Te 8 The N, P-C catalyst has higher catalytic activity and stability when catalyzing acidic methanol oxidation reaction.
Example 4
PtMo obtained in example 1 was tested separately 6 Te 8 N, P-C, ptMo obtained in example 2 6 Te 8 N-C and commerceApplication of Pt/C catalyst in acid electrolyte for catalyzing hydrogen evolution:
5mg of PtMo obtained in example 1 was taken 6 Te 8 N, P-C,5mg of PtMo obtained in example 2 6 Te 8 Respectively testing/N-C and 5mg commercial Pt/C catalyst, respectively adding three different catalysts into 950 mu L of anhydrous ethanol and 50 mu L of Nafion mixed solution, and uniformly dispersing by ultrasonic to obtain mixed solution; and (3) dropwise adding 10 mu L of the mixed solution onto the surface of a glassy carbon electrode to serve as a working electrode, a carbon rod to serve as a counter electrode and a Saturated Calomel Electrode (SCE) to serve as a reference electrode, placing the electrode into a sulfuric acid mixed system containing 1mol/L methanol and 0.5mol/L sulfuric acid, scanning by adopting a linear scanning voltammetry at a scanning speed of 5mV/s between 0 and-0.4V, and performing constant current timing test for 15 hours at a potential of-0.27V.
FIG. 4 shows PtMo 6 Te 8 /N,P-C、PtMo 6 Te 8 Linear sweep voltammograms and chronoamperometric test curves for N-C and commercial Pt/C catalysts in a 0.5mol/L sulfuric acid and 1mol/L methanol mixed solution. As can be seen from FIG. 4, ptMo 6 Te 8 N, P-C at 10mA cm drive -2 The minimum overpotential required at current density; after 15 hours of continuous stability test, the current density is hardly changed; compared with PtMo 6 Te 8 N-C and commercial Pt/C catalysts, ptMo of this invention 6 Te 8 The N, P-C catalyst has higher catalytic activity and stability when catalyzing acidic hydrogen evolution reaction.
Example 5
PtMo obtained in example 1 was tested separately 6 Te 8 Use of/N, P-C and commercial Pt/C catalysts in methanol electrolysis:
5mg of PtMo obtained in example 1 was taken 6 Te 8 Respectively testing/N, P-C and 5mg commercial Pt/C catalyst, respectively adding two different catalysts into 950 mu L of mixed solution of absolute ethyl alcohol and 50 mu L of Nafion, and uniformly dispersing by ultrasonic to obtain mixed solution; dripping 10 mu L of mixed solution on the surface of a glassy carbon electrode to serve as a cathode and an anode respectively, placing the electrode in a sulfuric acid mixed system containing 1mol/L methanol and 0.5mol/L sulfuric acid, and adopting a wireThe sexually scanned voltammetry was scanned at a scanning rate of 5mV/s between 0 and 1.25V and a constant current timing test was performed at a voltage of 0.72V for 20 hours.
FIG. 5 shows PtMo 6 Te 8 Linear sweep voltammogram and chronoamperometric test curves of/N, P-C and commercial Pt/C catalysts in methanol electrolysis. As can be seen from FIG. 5a, ptMo 6 Te 8 N, P-C as a dual-function catalyst for both cathode and anode, the voltage required for methanol electrolysis and water electrolysis is much less than for commercial Pt/C catalysts; as can be seen from FIG. 5b, ptMo after 20h of stability test 6 Te 8 The current density attenuation of the/N, P-C catalyst is less than that of the commercial Pt/C catalyst. Thus, ptMo of this invention 6 Te 8 The N, P-C catalyst has higher catalytic activity and stability in methanol electrolysis.
Claims (8)
1. The preparation method of the electro-catalyst for preparing hydrogen by methanol electrolysis is characterized in that molybdenum telluride doped with carbon by nitrogen and phosphorus is used as a composite carrier, and a carrier is platinum-based nano particles, and comprises the following steps:
(1) Dispersing molybdenum trioxide and imidazole in water, refluxing, naturally cooling to room temperature after refluxing, carrying out suction filtration, washing and vacuum drying to obtain Mo-MOF; uniformly mixing the prepared Mo-MOF and tellurium powder, and performing heat treatment under hydrogen-argon mixed gas to obtain nitrogen-doped carbon molybdenum telluride;
(2) Performing heat treatment on the molybdenum telluride doped with carbon by nitrogen and sodium hypophosphite in the step (1) under nitrogen to obtain molybdenum telluride doped with carbon by nitrogen and phosphorus;
(3) Adding the molybdenum telluride doped with carbon by nitrogen and phosphorus and the chloroplatinic acid aqueous solution in the step (2) into ethylene glycol, uniformly stirring, reducing platinum ions into a platinum simple substance by utilizing a microwave-assisted ethylene glycol reduction method, and after the reaction is finished, carrying out suction filtration, washing and vacuum drying to obtain the electrocatalyst of the molybdenum telluride loaded with carbon by nitrogen and phosphorus and platinum-based nano particles.
2. The electrocatalyst according to claim 1 wherein the loading of the platinum-based nanoparticles is from 20 to 60% of the total catalyst mass.
3. The electrocatalyst according to claim 1, wherein the platinum-based nanoparticles comprise elemental platinum or an alloy of platinum and a transition metal; wherein the transition metal comprises palladium, ruthenium, rhodium, silver, gold, cobalt or nickel.
4. The electrocatalyst according to claim 1 wherein the platinum-based nanoparticles have a particle size of from 1 to 10nm.
5. The electrocatalyst according to claim 1, wherein in step (1), the mass ratio of molybdenum trioxide to imidazole is 1 to 3:1, the reflux temperature is 100 to 130 ℃, and the reflux time is 10 to 20 hours.
6. The electrocatalyst according to claim 1, wherein in step (1), the mass ratio of Mo-MOF to tellurium powder is 1:0.5 to 2, the temperature rise rate is 2 to 10 ℃/min under the hydrogen-argon mixture, the heat treatment temperature is 800 to 1000 ℃, the heat treatment time is 1 to 3 hours, and the volume percentage of hydrogen in the hydrogen-argon mixture is 5 to 10%.
7. The electrocatalyst according to claim 1, wherein in step (2), the mass ratio of the nitrogen-doped molybdenum telluride to the sodium hypophosphite is 1:3-8, the temperature rise rate is 2-10 ℃/min under nitrogen, the heat treatment temperature is 150-350 ℃, and the heat treatment time is 1-3 hours.
8. The electrocatalyst according to claim 1 wherein in step (3) the microwave power is 500 to 800W and the microwave time is 2 to 5 minutes.
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