CN114029050B - Synthesis method of supported high-load carbon-coated noble metal nanoparticle catalyst - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000003054 catalyst Substances 0.000 title claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 30
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 30
- 239000002082 metal nanoparticle Substances 0.000 title claims abstract description 8
- 238000001308 synthesis method Methods 0.000 title abstract description 5
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 150000001768 cations Chemical class 0.000 claims abstract description 10
- 238000000197 pyrolysis Methods 0.000 claims abstract description 9
- 238000004108 freeze drying Methods 0.000 claims abstract description 8
- 239000003273 ketjen black Substances 0.000 claims abstract description 8
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 claims abstract description 5
- 229940082004 sodium laurate Drugs 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000011068 loading method Methods 0.000 abstract description 19
- 239000000243 solution Substances 0.000 abstract description 16
- 239000007864 aqueous solution Substances 0.000 abstract description 8
- 238000011065 in-situ storage Methods 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 7
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 abstract description 4
- DANYXEHCMQHDNX-UHFFFAOYSA-K trichloroiridium Chemical compound Cl[Ir](Cl)Cl DANYXEHCMQHDNX-UHFFFAOYSA-K 0.000 abstract description 4
- 229910021638 Iridium(III) chloride Inorganic materials 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 27
- 229910052697 platinum Inorganic materials 0.000 description 14
- 239000004115 Sodium Silicate Substances 0.000 description 8
- 235000019795 sodium metasilicate Nutrition 0.000 description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 8
- 229910052911 sodium silicate Inorganic materials 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 5
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 5
- 229910000457 iridium oxide Inorganic materials 0.000 description 5
- 229940070765 laurate Drugs 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 5
- 239000011943 nanocatalyst Substances 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 5
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 5
- POULHZVOKOAJMA-UHFFFAOYSA-M dodecanoate Chemical compound CCCCCCCCCCCC([O-])=O POULHZVOKOAJMA-UHFFFAOYSA-M 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- -1 ruthenium cation ion Chemical class 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 239000000969 carrier Substances 0.000 description 2
- 238000007385 chemical modification Methods 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000006181 electrochemical material Substances 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 244000195895 saibo Species 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/462—Ruthenium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/468—Iridium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
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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
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Abstract
The invention provides a synthesis method of a supported high-load carbon-coated noble metal nanoparticle catalyst, which comprises the following steps: dispersing the substrate in a sodium laurate aqueous solution, and ultrasonically stirring to uniformly disperse the substrate; adding noble metal cation solution, and freeze-drying; washing after high-temperature pyrolysis; wherein the substrate is graphene oxide or Ketjen black; the noble metal cation solution is platinum tetrachloride, ruthenium trichloride or iridium trichloride aqueous solution. The invention can grow a plurality of monodisperse high-load carbon-coated noble metal catalysts in situ on the substrate, and has the advantages of simple method, small catalyst particle size and high loading capacity. The problems of low loading capacity and high loading capacity of the noble metal catalyst in the prior art are solved, and the method for loading the noble metal with high loading capacity is expanded.
Description
Technical Field
The invention belongs to the field of materials and inorganic chemistry, in particular to a method for synthesizing a supported high-load carbon-coated noble metal nanoparticle catalyst, and particularly relates to a method for growing a high-load carbon-coated noble metal catalyst in situ on various carriers by utilizing surface chemical modification.
Background
With the proposition of the goal of "carbon peaking, carbon neutralization", fuel cells are coming up with new development opportunities. What is currently restricting the development of fuel cells is the preparation and loading of the catalyst. The current commercially available fuel cell ORR reaction catalysts are primarily platinum-based catalysts, while OER and HER catalysts are often ruthenium-based or iridium-based catalysts. In order to achieve the most efficient operation of the catalyst, the catalyst is often supported on a special carbon support.
There are two catalyst supporting methods, the first is to synthesize the noble metal nanoparticles first and then to support them on the carrier. The second is to introduce a metal precursor into the support and then grow in situ to obtain the catalyst. The second method has more commercial application prospect because of simple operation and clean catalyst surface.
However, in the existing noble metal catalyst in-situ growth loading technology, metal cations are usually adsorbed on a carrier and then reduced by a reducing agent, the loading capacity is low, catalyst agglomeration cannot be avoided when the loading capacity is increased, and residual organic matters are not removed well, so that the catalytic performance of the catalyst is influenced. Moreover, in order to achieve long-term use stability of the catalyst, the catalyst is often carbon-coated, so that the whole process is often complicated. Therefore, there is a need to develop a method capable of supporting a carbon-coated noble metal catalyst on a variety of carbon supports at high in-situ loadings in one step.
Disclosure of Invention
The technical purpose of the invention is to provide a synthesis method of a supported high-load carbon-coated noble metal nanoparticle catalyst, which can support a layer of noble metal catalyst on various carriers in a high-load manner through surface chemical modification.
The invention provides a synthesis method of a supported high-load carbon-coated noble metal nanoparticle catalyst, which comprises the following steps:
(1) Dispersing a substrate in a sodium laurate water solution, and performing ultrasonic stirring to uniformly disperse the substrate;
(2) Adding a noble metal cation solution into the solution obtained in the step (1), and then freeze-drying;
(3) Performing high-temperature pyrolysis on the product obtained in the step (2), and then washing the product to coat a layer of noble metal nano catalyst on the substrate;
wherein, the substrate in the step (1) can be graphene oxide or ketjen black; in the step (2), the noble metal cation solution is a platinum tetrachloride, ruthenium chloride or iridium chloride aqueous solution; in the step (3), under the condition of nitrogen atmosphere, the high-temperature pyrolysis is firstly carried out by 180-200 o 400-450 hours after C1-3 hours o And C, 2-3 hours, wherein the noble metal cation is reduced to carbon, and the laurate radical is converted to carbon, so that the clean noble metal catalyst surface is obtained.
In the invention, the mass ratio of the substrate to the sodium monthly silicate in the step (1) is 1.
In the invention, the mole ratio range of sodium metasilicate and platinum tetrachloride in the step (2) is as follows: 2:1-4:1.
In the invention, the mole ratio range of sodium metasilicate and ruthenium trichloride in the step (2) is as follows: 2:1-3:1.
In the invention, the molar ratio range of sodium metasilicate to iridium trichloride in the step (2) is as follows: 2:1-3:1.
According to the invention, sodium metasilicate is modified on the surfaces of various substrates in situ, then a noble metal cation aqueous solution is added, so that noble metal cations are fixed on the surface of a carrier, and then the carrier is coated with a layer of carbon-coated noble metal catalyst by freeze-drying and in-situ pyrolysis, without additionally adding a reducing agent.
The invention has the advantages that the invention can grow a plurality of monodisperse high-load carbon-coated noble metal catalysts in situ on the substrate, and the method is simple, the particle size of the catalyst is small, and the loading amount is high. The problems of low loading capacity and high loading capacity of the noble metal catalyst in the prior art are solved, and the method for loading the noble metal with high loading capacity is expanded.
Drawings
FIG. 1 is a transmission electron microscope image of the graphene loaded platinum prepared in example 1;
FIG. 2 is a transmission electron micrograph of graphene-supported ruthenium oxide prepared in example 2;
FIG. 3 is a transmission electron micrograph of the graphene-supported iridium oxide prepared in example 3;
FIG. 4 is a transmission electron micrograph of Ketjen black loaded with platinum obtained in example 4.
Detailed Description
Example 1
(1) 30 mg graphene oxide (institute of Chinese academy of sciences) is dispersed in 20 ml of 0.25 mol/L sodium metasilicate solution, and the solution is uniformly dispersed by ultrasonic treatment for 30 minutes and stirring for two hours.
(2) To the solution obtained in step (1), 1.5 ml of a 1 mol/L aqueous solution of platinum tetrachloride was slowly added, followed by lyophilization.
(3) And (3) pyrolyzing the precursor obtained in the step (2) at a high temperature, and then washing with water to obtain the graphene-supported platinum catalyst. The high-temperature pyrolysis condition is 180 ℃ under the nitrogen atmosphere o C3 h, 450 o C2 hours, at which point the platinum cationThe seed is reduced to carbon and the laurate is converted to carbon.
Fig. 1 is a transmission electron microscope image of the graphene-supported platinum catalyst prepared in example 1, and it can be seen that a layer of platinum particles with a diameter of about 3nm is coated on the surface of graphene, and the platinum particles are uniformly coated with carbon, which indicates that the method can load a layer of carbon-coated platinum nanocatalyst on the upper surface of graphene in a high loading manner.
Example 2
(1) 50 mg graphene oxide is dispersed in 20 ml of 0.25 mol/L sodium metasilicate solution, and the solution is ultrasonically treated for 30 minutes and stirred for two hours to uniformly disperse the graphene oxide.
(2) 2.5 ml of a 1 mol/L aqueous solution of ruthenium chloride was slowly added to the solution obtained in step (1), followed by lyophilization.
(3) And (3) pyrolyzing the precursor obtained in the step (2) at high temperature, and then washing with water to obtain the graphene-loaded ruthenium oxide catalyst. The high-temperature pyrolysis condition is a nitrogen atmosphere of 200 o C1 hour, 400 o C3 hours, at which time the ruthenium cation ion is reduced to carbon and the laurate is converted to carbon.
Fig. 2 is a transmission electron microscope image of the graphene-supported ruthenium oxide catalyst prepared in example 2, and it can be seen that the surface of graphene is coated with a layer of ruthenium oxide particles with a diameter of about 1nm, which indicates that the method can coat a layer of ruthenium oxide nano catalyst on the upper surface of graphene in a high loading manner.
Example 3
(1) dispersing 30 mg graphene oxide in 20 ml of 0.25 mol/L sodium metasilicate solution, and carrying out ultrasonic treatment for 30 minutes and stirring for two hours to uniformly disperse the graphene oxide.
(2) 2.5 ml of a 1 mol/L aqueous solution of iridium chloride was slowly added to the solution obtained in step (1), followed by lyophilization.
(3) And (3) pyrolyzing the precursor obtained in the step (2) at a high temperature, and washing with water to obtain the graphene supported eye iridium oxide catalyst. The high-temperature pyrolysis condition is nitrogen atmosphere 180 o C3 hours, 400 o And C3 hours, at which time the iridium cations are reduced to carbon and the laurate is converted to carbon.
Fig. 3 is a transmission electron microscope image of the graphene-supported iridium oxide catalyst prepared in example 3, and it can be seen that the surface of graphene is coated with a layer of iridium oxide particles with a diameter of about 1nm, which indicates that the method can coat a layer of iridium oxide nanocatalyst on the upper surface of graphene in a high loading manner.
Example 4
(1) 50 mg Ketjen black (Saibo electrochemical material net) was dispersed in 20 ml of 0.25 mol/L sodium metasilicate solution, and then uniformly dispersed by ultrasonic treatment for 30 minutes and stirring for two hours.
(2) To the solution obtained in step (1), 1.5 ml of a 1 mol/L aqueous solution of platinum tetrachloride was slowly added, followed by lyophilization.
(3) And (3) pyrolyzing the precursor obtained in the step (2) at high temperature, and then washing with water to obtain the Ketjen black supported platinum catalyst. The high-temperature pyrolysis condition is a nitrogen atmosphere of 200 o C2 hours, 400 o C3 hours, at which time the platinum cation is reduced to carbon and the laurate is converted to carbon.
Fig. 4 is a transmission electron microscope image of the ketjen black-supported platinum catalyst prepared in example 4, and it can be seen that the surface of the ketjen black is coated with a layer of platinum particles with a diameter of about 3nm, which indicates that the carrier is changed and then the carrier is still coated with a layer of platinum nano-catalyst in a high loading manner on the surface of the ketjen black.
Claims (2)
1. A method for synthesizing a supported high-load carbon-coated noble metal nanoparticle catalyst is characterized by comprising the following steps of:
(1) Dispersing a substrate in a sodium laurate water solution, and performing ultrasonic stirring to uniformly disperse the substrate; the mass ratio of the substrate to the sodium laurate is 1;
(2) Adding a noble metal cation solution into the solution obtained in the step (1), and then freeze-drying;
(3) Pyrolyzing the product obtained in the step (2) at high temperature and washing with water;
wherein, the substrate in the step (1) is graphene oxide or Ketjen black; in the step (2), the noble metal cation solution is platinum tetrachloride; and (3) heating at 180-200 ℃ for 1-3 hours and at 400-450 ℃ for 2-3 hours under the condition of nitrogen atmosphere in the high-temperature pyrolysis.
2. The process according to claim 1, characterized in that the molar ratio of sodium laurate to platinum tetrachloride in step (2) is in the range of: 2:1-4:1.
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