CN111834642B - Organic matter electrocatalytic oxidation catalyst and preparation method and application thereof - Google Patents
Organic matter electrocatalytic oxidation catalyst and preparation method and application thereof Download PDFInfo
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- CN111834642B CN111834642B CN201910297610.5A CN201910297610A CN111834642B CN 111834642 B CN111834642 B CN 111834642B CN 201910297610 A CN201910297610 A CN 201910297610A CN 111834642 B CN111834642 B CN 111834642B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses an organic electro-catalytic oxidation catalyst, and provides a preparation method of the catalyst and application of the catalyst in C, H, N, O micromolecule organic electro-catalytic oxidation. The catalyst is a transition metal compound loaded noble metal with a molecular formula of x1％M1 x2％M2 x3％M3/HyQaRbYcN3Wherein M is1、M2、M3Is a noble metal, x1％、x2％、x3% is the percentage content of noble metal in the total mass of the catalyst, wherein at most two values are 0, the rest values are 0.1-20%, Q, R, Y is transition metal, y value is 0-1, a + b + c is 1, N is one element of oxygen, nitrogen, carbon, phosphorus and sulfur. The organic electro-catalytic oxidation catalyst prepared by the method can greatly reduce the use amount of noble metals, can realize the decomposition of small molecules by repeatedly utilizing waste heat generated by the fuel cell, and improves the utilization rate of the fuel cell.
Description
Technical Field
The invention belongs to the field of catalysts, and particularly relates to an organic electro-catalytic oxidation catalyst, a preparation method thereof and application thereof in C, H, N, O micromolecular organic electro-catalytic oxidation.
Background
Hydrogen energy is the most ideal green energy source in the 21 st centuryHas the advantages of cleanness, high efficiency and high quality. C, H, N, O micromolecule liquid organic matters are used as fuel, so that the problems of storage, transportation and safety of hydrogen in the hydrogen fuel cell can be avoided. When the fuel cell works, C, H, N, O micromolecule liquid organic matters enter the flow channel from the anode flow field plate, then enter the anode catalyst through the anode diffusion layer, are oxidized under the action of the catalyst to release electrons and protons, and C, H, N, O micromolecule liquid organic matters after reaction are discharged from the anode. The electrons flow through an external circuit to do work, and the protons are transferred to the cathode through the solid electrolyte membrane. At the moment, oxygen or air enters the flow channel through the cathode flow field plate, enters the cathode catalyst layer through the cathode diffusion layer, and reacts with protons transferred from the anode in a combined manner to generate H2O, while consuming electrons transferred from the external circuit. Generation of H2O is discharged from the cathode in the form of water vapor or condensed water. At present, C, H, N, O catalysts for electrocatalytic oxidation of small-molecular organic matters are mainly precious metal materials such as Pd, Pt, Ru, Rh and the like, and are expensive and deficient in resources, so that development of a hydrogen production catalyst for electrolysis of water with low precious metal content, low cost and high efficiency is a research hotspot in the fields of energy, catalysis and materials.
Through long-term exploration and research, professor of Chenghangsong and teams thereof discover that a class of transition metal oxides has good addition/dehydrogenation performance and long cycle life, and the class of transition metal oxides becomes an electronic conductor after hydrogenation. The principle of electrocatalytic oxidation is similar to Hydrodeoxygenation (HDO), Hydrodenitrogenation (HDN) and Hydrodesulfurization (HDS), so that the material can be a high-efficiency and stable electrocatalytic oxidation catalyst.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides an organic electro-catalytic oxidation catalyst, a preparation method of the catalyst and application of the catalyst in the electro-catalytic oxidation of C, H, N, O small-molecule organic matters.
In order to achieve the purpose, the invention adopts the following technical scheme: an electrocatalytic oxidation catalyst for organic matters, which is a transition metal compound loaded noble metal and has a molecular formula of x1％M1 x2％M2 x3％M3/HyQaRbYcN3Wherein M is1、M2、M3Is a noble metal, x1％、x2％、x3% is the percentage content of noble metal in the total mass of the catalyst, wherein at most two values are 0, the rest values are 0.1-20%, Q, R, Y is transition metal, y value is 0-1, a + b + c is 1, N is one element of oxygen, nitrogen, carbon, phosphorus and sulfur.
Further, M1、M2、M3Is one of ruthenium, rhodium, palladium, osmium, iridium and platinum.
Further, Q, R, Y is one element selected from scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, niobium, molybdenum, rhodium, osmium, tungsten, tantalum, and iridium.
A preparation method of an organic electro-catalytic oxidation catalyst comprises the following steps:
(1) weighing two or three transition metal acid ammonium salts and polyethylene glycol, stirring and mixing, and heating and stirring the mixed solution; after stirring, dropwise adding 10% dilute nitric acid to adjust the pH of the solution to 1-3;
(2) filling the mixed solution into a hydrothermal reaction kettle for hydrothermal reaction; after the reaction is finished, carrying out suction filtration, washing the reactant to be neutral by using ultrapure water and ethanol, and fully drying at 60 ℃;
(3) calcining the dried product at high temperature for 1-5 h to obtain a metal oxide product;
(4) putting the product into a high-temperature high-pressure reaction kettle, and reacting to obtain transition metal oxide HxQaRbYcO3；
(5) The product H is reacted withxQaRbYcO3And NH3、H2/CH4、NaH2PO2Or calcining the sulfur powder at the high temperature of 350-700 ℃ for 2 hours to respectively prepare nitrogen, carbon, phosphorus and sulfide of the transition metal;
(6) charging noble metal salt and the transition metal oxygen, nitrogen, carbon, phosphorus or sulfide into round-bottom flask, adding ethylene glycol and water, ultrasonically dispersing, and introducing nitrogen gasReducing the mixture in an oil bath for 6 to 12 hours at 140 to 160 ℃ in the atmosphere, filtering, washing the reactant to be neutral by ultrapure water, and fully drying the reactant at 60 ℃ to obtain a transition metal compound supported noble metal x1％M1 x2％M2 x3％M3/HyQaRbYcN3。
Further, in the step 1, the mass ratio of the metal acid ammonium salt to the polyethylene glycol is 1:2,
further, in the step 1, the reaction conditions of the mixed solution are that the temperature is controlled to be 50-70 ℃, and the stirring time is controlled to be 24-72 hours.
Further, the hydrothermal reaction condition in the step 2 is that the temperature is 150-250 ℃, and the reaction time is 48-62 hours.
Further, the calcining temperature in the step 3 is 200-500 ℃.
Further, the reaction conditions of the step 4 are that the temperature is 150-500 ℃, the hydrogen pressure is 3MPa, and the heating reaction is carried out for 2-5 hours.
An application of organic electro-catalytic oxidation catalyst in the electro-catalytic oxidation reaction of small molecular organic matters.
The organic electro-catalytic oxidation catalyst prepared by the method can greatly reduce the use amount of noble metals, can realize the decomposition of small molecules by repeatedly utilizing waste heat generated by the fuel cell, and improves the utilization rate of the fuel cell.
Drawings
FIG. 1 is a diagram showing the construction of a test system according to example 3.
FIG. 2 is a polarization plot of the catalyst of example 3.
Detailed Description
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only partial embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that the terms "comprises" and "comprising," and any variations thereof, in the description and claims of this application and the above-described drawings, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
Example 1
(1) Weighing 10g of ammonium metatungstate and 10.8g of ammonium paramolybdate, stirring and mixing with polyethylene glycol, and stirring for 48h at 60 ℃; after stirring, dropwise adding dilute nitric acid with the mass ratio of 10% to adjust the pH of the solution to 2;
(2) filling the mixed solution into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 48 hours at the temperature of 200 ℃;
(3) after the hydrothermal reaction is finished, carrying out suction filtration, washing the reactant to be neutral by using ultrapure water and ethanol, and fully drying at 60 ℃;
(4) calcining the dried substance at high temperature for 5h to obtain a bimetal oxide product;
(5) putting the product into a high-temperature high-pressure reaction kettle, heating and reacting for 5 hours at the temperature of 150 ℃ and the hydrogen pressure of 3MPa to obtain H0.15Mo0.6W0.4O3。
(6) 100mg of the hydride was weighed into a round-bottomed flask, and 429. mu.L of 10mg/mL H was measured2PtCl6Putting the solution, 60mL of ethylene glycol and 40mL of ultrapure water into a round-bottom flask, performing ultrasonic dispersion for half an hour, stirring and performing oil bath reduction for 6 hours at 140 ℃ in a nitrogen atmosphere, performing suction filtration, washing a reactant to be neutral by using the ultrapure water, and sufficiently drying at 60 ℃ to obtain a binary transition metal oxide loaded noble metal 2% Pt/H0.15Mo0.6W0.4O3。
Example 2
(1) Weighing 10g of ammonium metatungstate, 10.8g of ammonium paramolybdate and 7.8g of nickel nitrate, stirring and mixing with polyethylene glycol, and stirring for 48h at 60 ℃; after stirring, dropwise adding dilute nitric acid with the mass ratio of 10% to adjust the pH of the solution to 2;
(2) filling the mixed solution into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 48 hours at the temperature of 200 ℃;
(3) after the hydrothermal reaction is finished, carrying out suction filtration, washing the reactant to be neutral by using ultrapure water and ethanol, and fully drying at 60 ℃;
(4) calcining the dried substance at high temperature for 5h to obtain a trimetal oxide product;
(5) putting the product into a high-temperature high-pressure reaction kettle, heating and reacting for 5 hours at the temperature of 150 ℃ and the hydrogen pressure of 3MPa to obtain H0.15Ni0.29Mo0.42W0.29O3；
(6) 100mg of the hydride was weighed into a round-bottomed flask, and 429. mu.L of 10mg/mL H was measured2PtCl6Solution, 168.3. mu.L of 10mg/mL PdCl2Putting the solution, 90mL of ethylene glycol and 60mL of ultrapure water into a round-bottom flask, performing ultrasonic dispersion for half an hour, stirring and performing oil bath reduction for 6 hours at 140 ℃ in a nitrogen atmosphere, performing suction filtration, washing a reactant to be neutral by using the ultrapure water, and sufficiently drying at 60 ℃ to obtain the ternary transition metal oxide loaded with the two noble metals, namely 2% Pt and 1% Pd/H0.15 Ni0.29Mo0.42W0.29O3。
Example 3
1. 2％Pt/H0.15Mo0.6W0.4O3Method for preparing catalyst solution
9.4mg of 2% Pt/H was weighed0.15Mo0.6W0.4O3The catalyst (hereinafter referred to as catalyst) is dispersed in the mixed solution of 4mL of absolute ethyl alcohol and 1mL of deionized water, 1.6mg of conductive carbon black is added, and the mixture is subjected to ultrasonic treatment for 1 hour to uniformly disperse the catalyst.
2. Method for spraying electrode
(1) And (3) carbon paper treatment: cutting carbon paper with the size of 2.0cm multiplied by 2.0cm, and blowing off pollutants such as impurities on the carbon paper by using an ear washing ball.
(2) Spraying of an electrode: and (3) placing the carbon paper in the step (1) on a sample table of an electrostatic spraying instrument, pouring the uniformly dispersed catalyst solution into a syringe, placing the syringe in a sample chamber, and adjusting the spraying voltage and the spraying flow rate to enable the carbon paper to be sprayed in a mist shape and uniformly sprayed on each part of the carbon paper. And naturally drying the prepared carbon paper for subsequent testing. The spraying of the catalyst of the anode and the cathode is respectively carried out by the method.
3. Electrocatalytic oxidation performance test
(1) Building a single battery test system: the single cell testing system mainly comprises a single cell system, a fuel feeding and discharging system, an oxygen or air feeding and discharging system, a temperature control system, a software control system and the like, and the structure of the single cell testing system is shown in figure 1.
(2) Testing the performance of the fuel cell: the fuel cell testing platform software control system is used for enabling the electronic load to work in a constant current mode, the load current is continuously changed to measure the output voltage value of the single cell under different current densities, and then the I-V curve of the single cell can be obtained through data processing and drawing. In the experimental process, the battery is heated through a temperature control system, the isopropanol micromolecule liquid organic matter is preheated through an oven, and the I-V curve test is carried out when the isopropanol micromolecule liquid organic matter is preheated to a set value. Setting the fuel flow to be 1mL/min, the oxygen flow to be 0.6mL/min, setting the current initial value to be 0A, setting the current final value based on the output voltage value to be 0.1V, setting each group of load current to correspond to the test time to be about 3min, stabilizing for 10s under the current load, and taking one group of data every 2 s. Selecting current density as gradient change according to polarization curve characteristics, sequentially increasing load current value until single cell voltage is reduced to about 0.1V, and finishing to obtain I-V curve as shown in FIG. 2, wherein the power density of the catalyst at 180 deg.C is 10mW/cm2(ii) a And after the experiment is finished, closing the test platform, discharging the isopropanol micromolecule organic solution in the pipeline, introducing nitrogen into the cathode of the single cell for purging, and closing the nitrogen after the cell is cooled to room temperature.
Although the present invention has been described with reference to the preferred embodiments, the embodiments and drawings are not intended to limit the present invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention should be defined by the claims of the present application.
Claims (8)
1. Is organicThe electrocatalytic oxidation catalyst is characterized in that: the catalyst is a transition metal compound loaded noble metal with a molecular formula of x1％M1 x2％M2 x3％M3/HyQaRbYcN3Wherein M is1、M2、M3Is a noble metal, x1％、x2％、x3% is the percentage content of noble metal in the total mass of the catalyst, wherein at most two values are 0, the rest values are 0.1-20%, Q, R, Y is transition metal, y is 0-1, a + b + c is 1, at most one value of a, b and c is zero, and N is one element of oxygen, nitrogen, carbon, phosphorus and sulfur;
the M is1、M2、M3Is one element of ruthenium, rhodium, palladium, osmium, iridium and platinum;
q, R, Y is one element selected from scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, niobium, molybdenum, rhodium, osmium, tungsten, tantalum and iridium.
2. A method for preparing an electrocatalytic oxidation catalyst for organic matter according to claim 1, comprising the steps of:
(1) weighing two or three transition metal acid ammonium salts and polyethylene glycol, stirring and mixing, and heating and stirring the mixed solution; after stirring, dropwise adding 10% dilute nitric acid to adjust the pH of the solution to 1-3;
(2) filling the mixed solution into a hydrothermal reaction kettle for hydrothermal reaction; after the reaction is finished, carrying out suction filtration, washing the reactant to be neutral by using ultrapure water and ethanol, and fully drying at 60 ℃;
(3) calcining the dried product at high temperature for 1-5 h to obtain a metal oxide product;
(4) putting the product into a high-temperature high-pressure reaction kettle, and reacting to obtain transition metal oxide HxQaRbYcO3；
(5) The product H is reacted withxQaRbYcO3And NH3、H2/CH4、NaH2PO2Or calcining the sulfur powder at the high temperature of 350-700 ℃ for 2 hours to respectively prepare nitrogen, carbon, phosphorus and sulfide of the transition metal;
(6) putting noble metal salt and the transition metal oxygen, nitrogen, carbon, phosphorus or sulfide into a round-bottom flask, adding ethylene glycol and water, ultrasonically dispersing, reducing in an oil bath at 140-160 ℃ in a nitrogen atmosphere for 6-12 h, performing suction filtration, washing reactants to be neutral by ultrapure water, and fully drying at 60 ℃ to obtain a transition metal compound loaded noble metal x1％M1 x2％M2 x3％M3/HyQaRbYcN3。
3. The method of claim 2, wherein: in the step 1, the mass ratio of the metal acid ammonium salt to the polyethylene glycol is 1: 2.
4. The method of claim 2, wherein: the reaction condition of the mixed solution in the step 1 is that the temperature is controlled to be 50-70 ℃, and the stirring time is controlled to be 24-72 hours.
5. The method of claim 2, wherein: the hydrothermal reaction condition in the step 2 is that the temperature is 150-250 ℃, and the reaction time is 48-62 h.
6. The method of claim 2, wherein: the calcination temperature in the step 3 is 200-500 ℃.
7. The method of claim 2, wherein: the reaction conditions of the step 4 are that the temperature is 150-500 ℃, the hydrogen pressure is 3MPa, and the heating reaction is carried out for 2-5 h.
8. The use of the organic electrocatalytic oxidation catalyst of claim 1 in electrocatalytic oxidation reactions of small molecular organic species.
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