CN108193500B - Composite nanofiber, composite nanofiber supported catalyst, preparation method and application thereof - Google Patents
Composite nanofiber, composite nanofiber supported catalyst, preparation method and application thereof Download PDFInfo
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- CN108193500B CN108193500B CN201611120356.4A CN201611120356A CN108193500B CN 108193500 B CN108193500 B CN 108193500B CN 201611120356 A CN201611120356 A CN 201611120356A CN 108193500 B CN108193500 B CN 108193500B
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/61—Polyamines polyimines
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- 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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- 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 provides a composite nanofiber and a composite nanofiber supported catalyst as well as preparation and application thereof.
Description
Technical Field
The invention relates to the technical field of fuel cells, in particular to a composite fiber electrocatalyst for a fuel cell and a preparation method thereof.
Background
Pt is the most common electrocatalyst of the proton exchange membrane fuel cell at present, wherein carbon-supported Pt (Pt/C) is the most widely used, however, the interaction force between Pt nano-ions and a carbon carrier is weak, and the carbon carrier is easy to corrode under high-temperature strong acid and strong electric field, thus the long-term operation stability of the fuel cell is seriously influenced.
To alleviate these problems, new supports are often used to prepare the catalysts. Metal oxides, especially low d-electron metal oxides such as TiO2And CeO2And the catalyst has excellent electric/chemical stability, acid and alkali corrosion resistance and catalytic increasing effect, has strong interaction with metal catalyst Pt to inhibit Pt agglomeration, and is concerned in preparing high-stability and high-catalytic-activity catalysts. But TiO22Poor conductivity, semiconductor characteristics of the electrons in Pt/TiO2The HOMO orbital energy of (A) is always lower than that of Pt/C, resulting in difficulty in electron transfer.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a metal oxide and conductive polymer composite nanofiber and a preparation method thereof, and accordingly, the invention provides a catalyst taking the composite nanofiber as a carrier and the preparation method thereof.
A composite nanofiber is a metal oxide nanofiber with a conductive polymer deposited on the surface, the composite nanofiber is microscopically a nanofiber net-shaped interwoven structure, and the diameter of the nanofiber is 50-500 nm; the mass content of the metal oxide in the composite nanofiber is 50-90%.
The conductive polymer is one or more than two of polyaniline, polypyrrole and polythiophene; the metal oxide is TiO2、CeO2、RuO2、SnO2One or a mixture of two or more of them.
The preparation method of the composite nanofiber comprises the following steps,
1) preparing an electrostatic spinning solution: preparing a polymer solution, adding precursor salt of the metal oxide into the obtained polymer solution, and uniformly mixing to obtain an electrostatic spinning solution;
2) preparation of metal oxide nanofibers: putting the electrostatic spinning solution obtained in the step 1) into electrostatic spinning equipment for spinning to obtain a metal oxide-polymer nanofiber precursor; carrying out heat treatment on the metal oxide-polymer nanofiber precursor at a certain temperature in the air or oxygen atmosphere to decompose the polymer to obtain the metal oxide nanofiber, wherein the certain temperature is the decomposition temperature of the polymer;
3) preparing composite nano fibers; dispersing the metal oxide nano-fiber obtained in the step 2) in a dilute acid solution to obtain a dispersion solution, sequentially adding a conductive polymer monomer solution and an oxidant into the dispersion solution, reacting at 0-4 ℃, washing and drying after the reaction is finished to obtain the composite nano-fiber.
The polymer solution in the step 1) is polyacrylonitrile or polyvinylpyrrolidone, and when the polymer is polyacrylonitrile, the solvent can be one or more than two of N, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide and dimethyl sulfoxide; when the polymer is polyvinylpyrrolidone, the solvent can be one or more than two of ethanol, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide and dimethyl sulfoxide; the mass fraction of the polymer in the polymer solution is 5-20%; the precursor salt of the metal oxide is one or a mixture of more than two of butyl titanate, cerium nitrate, ruthenium chloride and tin chloride; the mass fraction of the metal oxide precursor salt in the spinning solution is 5-20%;
the electrostatic spinning conditions of the step 2) are that the feeding speed of the electrostatic spinning solution is 0.03-1.0mm/min, the working voltage of the electrostatic spinning is 10-30kV, and the distance between the spinning needle head and the receiving part is 5-15 cm; the decomposition temperature of the polymer is 200-380 ℃;
the diluted acid solution in the step 3) is one or more than two of hydrochloric acid, sulfuric acid, phosphoric acid and perchloric acid, and the concentration is 0.5-2 mol/L; the conductive polymer monomer is one or more than two of aniline, pyrrole and thiophene acid; the oxidant is one of ammonium persulfate, potassium persulfate, hydrogen peroxide and ferric chloride; the molar ratio of the monomer to the oxidant is 1: 1-3.
The active component of the catalyst loaded by the composite nano-fiber is one or two of noble metals of Pt, Pd, Ru, Au and Ph, and the mass content of the active component in the catalyst is 10-40%.
The active component noble metal is loaded on the surface of the composite nanofiber in the form of nanoparticles, and the particle size of the noble metal nanoparticles is 1-5 nm.
The preparation method of the composite nanofiber electrocatalyst comprises the following steps,
1) preparing an electrostatic spinning solution: preparing a polymer solution, adding precursor salt of the metal oxide into the obtained polymer solution, and uniformly mixing to obtain an electrostatic spinning solution;
2) preparation of metal oxide nanofibers: putting the electrostatic spinning solution obtained in the step 1) into electrostatic spinning equipment for spinning to obtain a metal oxide-polymer nanofiber precursor; carrying out heat treatment on the metal oxide-polymer nanofiber precursor at a certain temperature in the air or oxygen atmosphere to decompose the polymer to obtain the metal oxide nanofiber, wherein the certain temperature is the decomposition temperature of the polymer;
3) preparing composite nano fibers; dispersing the metal oxide nano-fiber obtained in the step 2) in a dilute acid solution to obtain a dispersion, sequentially adding a conductive polymer monomer solution and an oxidant into the dispersion, reacting at 0-4 ℃, washing and drying to obtain a metal oxide-conductive polymer composite nano-fiber;
4) preparation of composite nanofiber supported catalyst: dispersing the metal oxide-conductive polymer composite nanofiber obtained in the step 3) into ethylene glycol, adding a noble metal precursor salt to obtain a catalyst precursor mixed solution, adjusting the pH value of the solution to 12-14, and reacting at 100-150 ℃ for 1-5 h; cooling, adjusting the pH value of the solution to 3-5, and sequentially filtering, washing and vacuum drying to obtain the composite nanofiber supported catalyst; the noble metal precursor salt is one or more than two of chloroplatinic acid, platinum acetylacetonate, ruthenium chloride, iridium chloride, palladium chloride and chloroauric acid.
Another preparation method of the composite nano-fiber electrocatalyst comprises the following steps,
1) preparing an electrostatic spinning solution: preparing a polymer solution, adding precursor salt of the metal oxide into the obtained polymer solution, and uniformly mixing to obtain an electrostatic spinning solution;
2) preparation of metal oxide nanofibers: putting the electrostatic spinning solution obtained in the step 1) into electrostatic spinning equipment for spinning to obtain a metal oxide-polymer nanofiber precursor; carrying out heat treatment on the metal oxide-polymer nanofiber precursor at a certain temperature in the air or oxygen atmosphere to decompose the polymer to obtain the metal oxide nanofiber, wherein the certain temperature is the decomposition temperature of the polymer;
3) preparing a composite nanofiber supported catalyst; dispersing the metal oxide nano-fiber obtained in the step 2) in a dilute acid solution to obtain a dispersion solution, sequentially adding a conductive polymer monomer solution and a noble metal precursor salt solution into the dispersion solution, reacting at the temperature of 10-40 ℃, washing and drying to obtain the catalyst supported by the composite nano-fiber.
In the above two methods for preparing the composite nanofiber supported catalyst,
the polymer solution in the step 1) is polyacrylonitrile or polyvinylpyrrolidone, and when the polymer is polyacrylonitrile, the solvent can be one or more than two of N, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide and dimethyl sulfoxide; when the polymer is polyvinylpyrrolidone, the solvent can be one or more than two of ethanol, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide and dimethyl sulfoxide; the mass fraction of the polymer in the polymer solution is 5-20%; the precursor salt of the metal oxide is one or a mixture of more than two of butyl titanate, cerium nitrate, ruthenium chloride and tin chloride; the mass fraction of the metal oxide precursor salt in the spinning solution is 5-20%;
the electrostatic spinning conditions of the step 2) are that the feeding speed of the electrostatic spinning solution is 0.03-1.0mm/min, the working voltage of the electrostatic spinning is 10-30kV, and the distance between the spinning needle head and the receiving part is 5-15 cm; the decomposition temperature of the polymer is 200-380 ℃;
the diluted acid solution in the step 3) is one or more than two of hydrochloric acid, sulfuric acid, phosphoric acid and perchloric acid, and the concentration is 0.5-2 mol/L; the conductive polymer monomer solution is one or more than two of aniline, pyrrole and thiophene acid; the molar ratio of one monomer of ammonium persulfate, potassium persulfate, hydrogen peroxide and ferric chloride to the oxidant is 1: 1-3.
The invention aims at the defects of the prior art, invents a metal oxide and conductive polymer composite nanofiber and thereby invents a catalyst taking the composite nanofiber as a carrier. When the catalyst is used as an electrocatalyst for a fuel cell, the defects of easy corrosion of a carbon carrier and insufficient conductivity of a metal oxide carrier in the prior art are overcome. In addition, the composite fiber is prepared by combining an electrostatic spinning technology and a solution method, and the supported catalyst is further prepared by adopting a glycol reduction method and a solution method for direct reduction, the method is simple and easy to realize, and the activity and the performance of the prepared electrocatalyst are improved.
Drawings
FIG. 1 example1 electrospinning of the resulting TiO2Electron microscopy of nanofibers;
FIG. 2 an electron micrograph of an electrocatalyst prepared in example 1;
FIG. 3 an electron micrograph of an electrocatalyst prepared in example 2;
figure 4 XRF characterization of the electrocatalyst prepared in example 2.
Detailed Description
The preparation of the metal oxide-conductive polymer-Pt electrocatalyst prepared by the invention comprises the following steps: firstly, preparing a metal oxide fiber substrate by an electrostatic spinning method; there are then two ways to introduce the conductive polymer and Pt: one is to deposit conductive polymer on the surface of metal oxide, and then obtain Pt by using glycol solution reduction method; the other method is that Pt precursor salt is reduced into Pt while conductive polymer is introduced to modify the surface of the metal oxide fiber.
The present invention is carried out by the following embodiments, but the present invention is not limited to the following embodiments.
Example 1
Weighing 1g of polyvinylpyrrolidone, dissolving in 10g of ethanol, adding 3g of acetic acid, then adding 1.5g of butyl titanate, stirring for 1h to obtain a light yellow transparent spinning solution, standing, defoaming, moving into an injector, fixing on a workbench for electrostatic spinning, wherein the distance between the workbench and a roller or a stainless steel flat plate is 10cm, the feeding speed of the spinning solution is 0.04mm/min, applying a working voltage of 20kV, and fixing aluminum foil paper on the roller for collecting fibers, wherein the rotating speed of the roller is 120 rpm. Finally, the fiber is taken down from the aluminum foil paper and is put into a muffle furnace to be calcined for 4 hours at the temperature of 600 ℃ to obtain titanium oxide (TiO)2) And (3) nano fibers. FIG. 1 shows the TiO obtained2Electron microscopy of nanofibers.
Immersing the metal oxide fiber prepared by the electrostatic spinning method into 1M dilute hydrochloric acid solution, then adding aniline acid solution, and then adding oxidant ammonium persulfate acid solution, wherein the mass ratio of aniline to ammonium persulfate is 1:1, the two solutions are mixed quickly and then placed in a refrigerator to react for 24h at 4 ℃, and then the obtained product is washed by water to remove acid to be neutral and is vacuumizedDrying at 80 ℃ in a drying oven for 12h to remove water to finally obtain TiO2-PANI composite fibres.
Subsequently, 60mg of TiO were added2Dispersing the-PANI composite nano-fiber into 100mL of glycol solution, adding 3mL of chloroplatinic acid/glycol solution (7.5mgPt/mL), adjusting the pH value to 13 with sodium hydroxide glycol solution, stirring at 130 ℃ for reaction for 3h, cooling, adjusting the pH value to 4 with hydrochloric acid solution, continuing stirring for 1h, cooling to room temperature, filtering, washing and drying to obtain TiO2-PANI-Pt electrocatalyst. Fig. 2 is an electron micrograph of the resulting electrocatalyst.
Example 2
The TiO is obtained by electrostatic spinning in the same way as in example 12The nano-fiber is then weighed to obtain 100mg TiO2The fibers were dispersed in a 1M perchloric acid solution, 5mL of an aniline monomer solution (aniline monomer dissolved in perchloric acid, 0.05mol/L) was added thereto, and stirring was carried out, followed by 5mL of chloroplatinic acid (5mg of chloroplatinic acid dissolved in 50mg of water) and finally reaction was carried out at room temperature for 24 hours with stirring. The product was then washed with water to neutrality and dried in a vacuum oven at 80 ℃ for 12h to remove water. The resulting TiO2The morphology of the-PANI-Pt is shown in a projection electron microscope image shown in FIG. 3, and Pt nano particles are uniformly distributed on the surface of the carrier. To further characterize the resulting catalyst, X-ray fluorescence analysis was performed, as shown in fig. 4, to demonstrate the presence of surface Pt.
Comparative example
60mg of TiO2 nanoparticles are weighed and dispersed into 100mL of ethylene glycol solution, and Pt nanoparticles are introduced to the surface of TiO2 nanoparticles by the same ethylene glycol reduction method as in example 1 to prepare the TiO2-Pt catalyst.
The conductivity of the electrocatalyst support was tested with a four-probe method, where the conductivity of the TiO2 nanoparticles was <10-11S/cm, whereas the conductivity of the TiO2-PANI nanofiber support of example 1 was 0.16S/cm. In addition, the electrochemical specific surface area (ECSA) of the catalyst was measured by cyclic voltammetry, and the ECSA of the TiO2-Pt nanoparticle catalyst prepared by the conventional method was about 18m2g-1Pt, the ECSA of the electrocatalyst prepared in example 1 was about 44m2g-1Pt, and the ECSA of the electrocatalyst prepared in example 2 was about 56m2g-1 Pt. The performance of the prepared electro-catalyst is improved due to the improvement of the conductivity of the carrier on one hand, and the dispersion of Pt is improved due to the TiO2 nano carrier modified by the conductive polymer on the other hand.
Claims (9)
1. A composite nanofiber supported catalyst characterized by: the active component of the catalyst loaded by the composite nano-fiber is one or more than two of noble metals of Pt, Pd, Ru, Au and Ph, and the mass content of the active component in the catalyst is 10-40%;
the composite nanofiber is a metal oxide nanofiber with a conductive polymer deposited on the surface, the composite nanofiber is a nanofiber interwoven net structure on the micro scale, and the diameter of the nanofiber is 50-500 nm; the mass content of the metal oxide in the composite nanofiber is 50-90%;
the conductive polymer is one or more than two of polyaniline, polypyrrole and polythiophene; the metal oxide is TiO2、CeO2、RuO2、SnO2One or a mixture of two or more of them.
2. The composite nanofiber supported catalyst of claim 1, wherein: the active component noble metal is loaded on the surface of the composite nanofiber in the form of nanoparticles, and the particle size of the noble metal nanoparticles is 1-5 nm.
3. A method of preparing the composite nanofiber supported catalyst of claim 1, characterized by: comprises the following steps of (a) carrying out,
1) preparing an electrostatic spinning solution: preparing a polymer solution, adding precursor salt of the metal oxide into the obtained polymer solution, and uniformly mixing to obtain an electrostatic spinning solution;
2) preparation of metal oxide nanofibers: putting the electrostatic spinning solution obtained in the step 1) into electrostatic spinning equipment for spinning to obtain a metal oxide-polymer nanofiber precursor; carrying out heat treatment on the metal oxide-polymer nanofiber precursor at a certain temperature in the air and/or oxygen atmosphere to decompose the polymer to obtain the metal oxide nanofiber, wherein the certain temperature is the decomposition temperature of the polymer;
3) preparing composite nano fibers; dispersing the metal oxide nano-fiber obtained in the step 2) in a dilute acid solution to obtain a dispersion, sequentially adding a conductive polymer monomer solution and an oxidant into the dispersion, reacting at 0-4 ℃, washing and drying to obtain a metal oxide-conductive polymer composite nano-fiber;
4) preparation of composite nanofiber supported catalyst: dispersing the metal oxide-conductive polymer composite nanofiber obtained in the step 3) into ethylene glycol, adding a noble metal precursor salt to obtain a catalyst precursor mixed solution, adjusting the pH value of the solution to 12-14, and reacting at 100-150 ℃ for 1-5 h; cooling, adjusting the pH value of the solution to 3-5, and sequentially filtering, washing and vacuum drying to obtain the composite nanofiber supported catalyst; the noble metal precursor salt is one or more than two of chloroplatinic acid, platinum acetylacetonate, ruthenium chloride, iridium chloride, palladium chloride and chloroauric acid.
4. A method of preparing the composite nanofiber supported catalyst of claim 1, characterized by: comprises the following steps of (a) carrying out,
1) preparing an electrostatic spinning solution: preparing a polymer solution, adding precursor salt of the metal oxide into the obtained polymer solution, and uniformly mixing to obtain an electrostatic spinning solution;
2) preparation of metal oxide nanofibers: putting the electrostatic spinning solution obtained in the step 1) into electrostatic spinning equipment for spinning to obtain a metal oxide-polymer nanofiber precursor; carrying out heat treatment on the metal oxide-polymer nanofiber precursor at a certain temperature in the air and/or oxygen atmosphere to decompose the polymer to obtain the metal oxide nanofiber, wherein the certain temperature is the decomposition temperature of the polymer;
3) preparing a composite nanofiber supported catalyst; dispersing the metal oxide nano-fiber obtained in the step 2) in a dilute acid solution to obtain a dispersion solution, sequentially adding a conductive polymer monomer solution and a noble metal precursor salt solution into the dispersion solution, reacting at the temperature of 10-40 ℃, washing and drying to obtain the catalyst supported by the composite nano-fiber.
5. The method of preparing the composite nanofiber supported catalyst according to claim 3 or 4, wherein:
the polymer solution in the step 1) is polyacrylonitrile or polyvinylpyrrolidone, and when the polymer is polyacrylonitrile, the solvent is one or more than two of N, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide and dimethyl sulfoxide; when the polymer is polyvinylpyrrolidone, the solvent is one or more than two of ethanol, N-dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide and dimethyl sulfoxide; the mass fraction of the polymer in the polymer solution is 5-20%; the precursor salt of the metal oxide is one or a mixture of more than two of butyl titanate, cerium nitrate, ruthenium chloride and tin chloride; the mass fraction of the metal oxide precursor salt in the spinning solution is 5-20%.
6. The method of preparing the composite nanofiber supported catalyst according to claim 3 or 4, wherein:
the electrostatic spinning conditions of the step 2) are that the feeding speed of the electrostatic spinning solution is 0.03-1.0mm/min, the working voltage of the electrostatic spinning is 10-30kV, and the distance between the spinning needle head and the receiving part is 5-15 cm; the polymer decomposition temperature is 200-380 ℃.
7. A method of preparing the composite nanofiber supported catalyst of claim 3, wherein:
the diluted acid solution in the step 3) is one or more than two of hydrochloric acid, sulfuric acid, phosphoric acid and perchloric acid, and the concentration is 0.5-2 mol/L; the conductive polymer monomer solution is one or more than two of aniline, pyrrole and thiophene acid; the oxidant is one of ammonium persulfate, potassium persulfate, hydrogen peroxide and ferric chloride; the molar ratio of the monomer to the oxidant is 1: 1-3.
8. The method of preparing the composite nanofiber supported catalyst of claim 4, wherein:
the diluted acid solution in the step 3) is one or more than two of hydrochloric acid, sulfuric acid, phosphoric acid and perchloric acid, and the concentration is 0.5-2 mol/L; the conductive polymer monomer solution is one or more than two of aniline, pyrrole and thiophene acid.
9. Use of the composite nanofiber supported catalyst of any of claims 1-2, wherein: the catalyst is a fuel cell catalyst.
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| CN110424063B (en) * | 2019-08-25 | 2022-03-25 | 天津大学 | Preparation method of chemical fiber for catalyzing atomic-level sites of malodorous gas at normal temperature |
| CN111560665B (en) * | 2020-04-24 | 2021-12-14 | 中国科学院化学研究所 | Pt-loaded B and N co-doped In2O3/TiO2Nano fiber and preparation method and application thereof |
| CN112853751B (en) * | 2021-01-14 | 2021-11-26 | 天津大学 | Phenanthroline palladium functionalized fiber and preparation method and application thereof |
| CN113413894B (en) * | 2021-06-24 | 2023-04-07 | 兰州交通大学 | Preparation method of zinc ferrite electrostatic spinning membrane with photocatalytic antibacterial performance |
| CN114534797B (en) * | 2022-03-09 | 2024-02-27 | 东南大学 | Continuous flow purification and separation method of nanofiber supported catalyst |
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