CN111135840B - Preparation method of supported monatomic dispersed noble metal catalyst - Google Patents
Preparation method of supported monatomic dispersed noble metal catalyst Download PDFInfo
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- CN111135840B CN111135840B CN201811313889.3A CN201811313889A CN111135840B CN 111135840 B CN111135840 B CN 111135840B CN 201811313889 A CN201811313889 A CN 201811313889A CN 111135840 B CN111135840 B CN 111135840B
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8906—Iron and noble metals
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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
- 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
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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
- 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
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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
- 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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
Abstract
The invention discloses a preparation method of a supported monatomic dispersed noble metal catalyst, which is prepared by impregnating a noble metal precursor and carrying out pretreatment and activation and comprises the following steps: (1) dissolving a noble metal precursor in deionized water or a common organic solvent, and then adding a proper amount of common N, P, S-containing inorganic and organic reagents to obtain a noble metal precursor complex solution (the mass concentration of the noble metal is 0.0001-5%). (2) Soaking a certain amount of carrier in the noble metal precursor complex solution, stirring for 1-600 min, filtering, and drying at 60-120 deg.C for 6-12 hr to obtain noble metal catalyst precursor; (3) placing a certain amount of the catalyst precursor in He, Ar and N2、H2、O2And treating in air or other atmosphere at 200-800 deg.c for 10-600 sec to obtain the supported monoatomic dispersed noble metal catalyst. The noble metal in the catalyst of the invention exists in a form of high dispersion even atomic level dispersion, and the preparation process is simple, the utilization rate of metal atoms can reach 100 percent, and the catalyst is beneficial to large-scale application in industrial production.
Description
Technical Field
The invention belongs to the technical field of catalysts, and relates to a preparation method of a supported monatomic dispersed noble metal catalyst.
Background
One of the main research contents in catalytic processes is the development of efficient catalysts. Supported noble metal catalysts are widely used in many important industrial catalytic reactions due to their excellent catalytic properties. In the catalytic engineering of the supported catalyst, the catalytic performance is closely related to the size of the metal active component on the carrier. Namely, the size of the metal particles can be reduced, the utilization rate of metal atoms can be improved, and the catalytic activity of the catalyst can be further improved. In order to optimize the catalytic effect of each metal atom on a supported metal catalyst, researchers have continually reduced the particle size of the metal. Theoretically, the limit of dispersion (100% dispersion) of the supported metal catalyst is that the metal is uniformly distributed on the support in the form of a single atom. The ideal state of this supported metal catalyst brings the catalytic science into a smaller research scale, monatomic catalysis. Meanwhile, in the monatomic catalyst, particularly the noble metal catalyst, each metal atom is 'in one place of ten', which is beneficial to large-scale application in industrial production. Many patents and literature describe the preparation of different monatomic catalysts.
Document 1(Nature Chemistry,2011,3,634) prepares Pt by a coprecipitation method1The catalyst is found to be used in CO oxidation and PROX reaction, and single atom Pt1/FeOxThe catalyst shows high activity, 2-3 times higher than that of Pt sub-nanocluster catalyst.
Document 2(Journal of the American Chemical Society,2013,135,15314) prepares Ir by the coprecipitation method1The activity of the catalyst in the water-vapor shift reaction is higher by one order of magnitude than that of an Ir cluster or Ir nano particle catalyst, even higher than that of Au and Pt-based catalysts with the best activity. And proves that the single atom in the catalyst is the most main active site of the water-vapor shift reaction.
Document 3(Scientific Reports,2013,3,1775) prepares a Pt catalyst on graphene by using an atomic layer deposition method, and Pt nanoparticles, sub-nanoclusters and monatomic catalysts can be obtained by accurately adjusting and controlling preparation conditions. The monatomic Pt catalyst showed the best activity in the direct methanol fuel cell reaction, 10 times that of the commercial Pt/C catalyst.
Document 4(Journal of the american Chemical Society,2015,137,10484) prepared by loading Pd on a graphene support using an atomic layer deposition method, produced a Pd monatomic catalyst that was found to exhibit very good 1, 3-butadiene selective hydrogenation catalytic performance, and butene selectivity could reach 100% when the 1, 3-butadiene conversion was 95%.
Document 5(Science,2014,346,1498) prepares stably existing Au monoatomic atoms on MCM-41 and KLTL molecular sieve supports, respectively, by grinding and mixing a mesoporous silica support with an active component precursor, and a precursor of an alkaline ion (Na or K). Combining the results of experiments and theoretical calculations, the authors found that the Au monoatomic atom is stably present because of the Au-O (OH) x-Na (or K) structure formed between Au and the carrier. The authors have also found that these Au monatomic catalysts exhibit very good low temperature catalytic activity for the water gas shift reaction.
Document 6(Science,2014,344,616) prepares an Fe monatomic catalyst using SiC as a carrier, and this catalyst realizes the first highly selective production of ethylene and aromatic hydrocarbons from natural gas under oxygen-free conditions. The Fe monatomic structure avoids the coupling of C-C bonds and the generation of carbon deposition in the catalytic reaction process, so that the catalyst has very good stability. The conversion rate of methane in the reaction can reach 48.1%, and the selectivity of ethylene in the product can reach 48.4%. By testing their stability, the authors found that no significant deactivation of the catalyst occurred after 60 h.
Disclosure of Invention
The invention discloses a preparation method of a supported monatomic dispersed noble metal catalyst, and provides a novel universal preparation method of a high-dispersion noble metal catalyst, through which a noble metal catalyst with 100% metal dispersion degree, namely a monatomic catalyst, can be prepared, and the method opens up a new path for the application of the monatomic catalyst in industry.
In order to achieve the purpose, the invention adopts the technical scheme that the preparation method of the supported monatomic dispersion noble metal catalyst comprises a carrier and an active component, wherein the active component is common noble metal, the dispersion degree of the active component can reach atomic level dispersion, and the carrier is one or more than two of oxide or carbon materials. The mass content of the active component in the catalyst is 0.1-10%.
The preparation process of the catalyst comprises the following steps:
step 1: one or more than two of noble metal precursors (chloride, nitrate and organic complex) are used as noble metal sources, a certain amount of noble metal precursors are dissolved in deionized water or common organic solution, and a proper amount of common N, P, S-containing inorganic and organic reagents are added to obtain noble metal precursor complex solution.
Common organic solvents are: one or more than two of methanol, ethanol, acetone, toluene, dichloromethane, tetrahydrofuran, n-hexane, isopropanol, DMF, DMSO, acetonitrile or other organic solvents are mixed in any ratio.
The common inorganic reagent is one or a mixture of more than two of ammonia water, ammonium nitrate, ammonium chloride, ammonium carbonate, ammonium sulfate, ammonium sulfite, ammonium phosphate, ammonium phosphite or other N, P, S-containing inorganic reagents in any ratio.
The organic reagent is one or a mixture of more than two of ethylenediamine, diethylamine, ethanolamine, aniline, acetamide, EDTA, triphenylphosphine, triethyl phosphate, cystine, cysteine or other organic N, P, S-containing reagents in any ratio.
Step 2: common oxide or carbon material is used as carrier to be dipped into the noble metal precursor complex solution, and the carrier is stirred for 1 to 300 minutes, filtered and dried for 6 to 12 hours at the temperature of 60 to 120 ℃ to obtain the load type monoatomic dispersion noble metal catalyst precursor.
Common oxides are: one or more than two of aluminum oxide, silicon oxide, iron oxide, cerium oxide and titanium oxide in any ratio.
Common carbon materials are: activated carbon, acetylene black, mesoporous carbon material (CMK-3 and the like), graphene oxide, reduced graphene and C3N4One or more than two of them.
And step 3: placing the supported monoatomic noble metal catalyst precursor in a quartz tube, and adding He, Ar and N2、H2、O2And treating in air and other atmosphere at 200-800 deg.c for 10-600 sec to obtain the supported monoatomic dispersed noble metal catalyst.
The invention has the following effects:
by the method, the high-dispersion noble metal catalyst with metal atoms capable of reaching 100% can be obtained, and each metal atom is an active site, so that the method is favorable for large-scale application in industrial production. The invention provides a preparation method of a novel universal supported atomic-level dispersed noble metal catalyst, and opens up a new path for the application of a single-atom catalyst in industry.
The noble metal in the catalyst of the invention exists in a form of high dispersion even atomic level dispersion, and the preparation process is simple, the utilization rate of metal atoms can reach 100 percent, and the catalyst is beneficial to large-scale application in industrial production.
Drawings
FIG. 1 is an electron microscope picture of an atomically dispersed Pt-FeOx catalyst prepared by the method of the present invention.
FIG. 2 is an electron microscope picture of the atomically dispersed Pt-C catalyst prepared by the method of the present invention.
FIG. 3 is an electron microscope picture of the atomically dispersed Ru-C catalyst prepared by the method of the invention.
FIG. 4 is an electron microscope picture of the atomically dispersed Pt-C catalyst prepared by the method of the present invention.
FIG. 5 is an electron microscope picture of an atomically dispersed Pt-C catalyst prepared by the method of the present invention.
FIG. 6 is an electron microscope picture (comparative example) of Pt-FeOx supported nano-catalyst that was not prepared by the method of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and detailed description, but the invention is not limited thereto.
Example 1: 0.027g of chloroplatinic acid is dissolved in 10g of deionized water, 1g of 25% ammonia water is added, stirring is carried out for 2h, 1g of ferric oxide is added, stirring is carried out for 7h, filtering and washing are carried out, the mixture is placed in a drying oven at 60 ℃ and dried for 12h to obtain a load type monoatomic dispersion platinum-based catalyst precursor, the precursor is placed in a quartz tube, and the precursor is treated at 500 ℃ for 10 seconds under the He condition to obtain 1% Pt/FeOx catalyst which is placed in a dryer for standby. (catalyst electron microscope picture is shown in FIG. 1)
Example 2: 0.027g of chloroplatinic acid is dissolved in 10g of deionized water, 1g of ethylenediamine organic reagent is added, the mixture is stirred for 1 hour, 1g of activated carbon is added, the mixture is stirred for 6 hours, filtered and washed, the obtained product is placed in an oven at 80 ℃, the obtained product is dried for 10 hours to obtain a supported monoatomic dispersion platinum-based catalyst precursor, the precursor is placed in a quartz tube, and the obtained product is treated at 600 ℃ for 60 seconds under the He condition to obtain a 1% Pt/C catalyst which is placed in a dryer for standby. (catalyst electron microscope picture is shown in FIG. 2)
Example 3: 0.027g of chloroplatinic acid is dissolved in 10g of deionized water, 1.5g of ammonium nitrate is added, stirring is carried out for 2h, 1g of aluminum oxide is added, stirring is carried out for 4h, filtering and washing are carried out, the mixture is placed in a drying oven at 60 ℃, drying is carried out for 12h to obtain a load type monoatomic dispersion platinum-based catalyst precursor, the precursor is placed in a quartz tube, and after treatment is carried out for 240 seconds at 500 ℃ under Ar condition, 1% Pt/Al is obtained2O3And (5) putting the catalyst in a dryer for later use.
Example 4: 0.017g of palladium chloride is dissolved in 10g of ethanol, 2g of triethyl phosphate organic reagent is added, the mixture is stirred for 2 hours, 1g of ferric oxide is added, the mixture is stirred for 8 hours, filtered and washed, the mixture is placed in an oven at 80 ℃ and dried for 10 hours to obtain a supported monoatomic dispersion palladium-based catalyst precursor, the precursor is placed in a quartz tube, and the precursor is treated for 30 seconds at 550 ℃ under Ar condition to obtain 1% Pd/FeOx catalyst which is used in a dryer for standby.
Example 5: dissolving 0.021g of chloroauric acid in 10g of methanol, adding 0.5g of diethylamine organic reagent, stirring for 2h, adding 1g of cerium oxide, stirring for 6h, filtering, washing, drying in 70 ℃ oven for 12h to obtain a supported monoatomic dispersed gold-based catalyst precursor, placing the precursor in a quartz tube, and adding N2Processing at 550 ℃ for 300 seconds under the condition to obtain 1 percent Au/CeO2And (5) putting the catalyst in a dryer for later use.
Example 6: dissolving 0.027g chloroplatinic acid in 10g deionized water, adding 0.5g cystine organic reagent, stirring for 2h, adding 1g activated carbon, stirring for 6h, filtering, washing, placing in an oven at 80 deg.C, drying for 12h to obtain a supported monoatomic dispersed platinum-based catalyst precursor, and mixing the precursor with waterThe body is placed in a quartz tube, N2Treating at 500 deg.c for 120 sec to obtain 1% Pt/C catalyst in a drier for further use.
Example 7: 0.021g of dodecacarbonyl triruthenium is dissolved in 10g of acetone, 0.5g of 25% ammonia water is added, the mixture is stirred for 2 hours, 1g of activated carbon is added, the mixture is stirred for 6 hours, filtered and washed, the obtained product is placed in an oven at 80 ℃ and dried for 12 hours to obtain a supported monoatomic dispersion ruthenium-based catalyst precursor, the precursor is placed in a quartz tube, and the obtained product is treated at 500 ℃ for 60 seconds under Ar condition to obtain 1% Ru/C catalyst, and the obtained product is placed in a dryer for standby. (catalyst electron microscope picture is shown in FIG. 3)
Example 8: dissolving 0.135g of chloroplatinic acid in 10g of deionized water, adding 1g of ethylenediamine, stirring for 2h, adding 1g of activated carbon, stirring for 4h, filtering, washing, placing in an oven at 80 ℃, drying for 8h to obtain a supported monoatomic dispersed platinum-based catalyst precursor, placing the precursor in a quartz tube, treating at 600 ℃ under the He condition for 55 seconds to obtain a 5% Pt/C catalyst, and placing in a dryer for later use. (catalyst electron microscope picture is shown in FIG. 4)
Example 9: dissolving 0.27g of chloroplatinic acid in 10g of deionized water, adding 3g of diethylamine, stirring for 6h, adding 1g of activated carbon, stirring for 4h, filtering, washing, placing in a 70 ℃ oven, drying for 7h to obtain a supported monoatomic dispersed platinum-based catalyst precursor, placing the precursor in a quartz tube, treating at 600 ℃ under the He condition for 40 seconds to obtain a 10% Pt/C catalyst, and placing in a dryer for later use. (catalyst electron microscope picture is shown in FIG. 5)
Example 10 (comparative): 0.027g of chloroplatinic acid is dissolved in 1.5g of deionized water, 1g of ferric oxide is added, the mixture is stirred for 1 hour, the mixture is placed in an oven with the temperature of 120 ℃, dried for 6 hours and then placed in a quartz tube, and H2Processing for 300 seconds at 600 ℃ under the condition to obtain the 1 percent Pt/FeOx supported nano catalyst. (catalyst electron microscope picture is shown in FIG. 6)
As can be seen from fig. 1-5: the noble metal in the catalyst of the invention exists in a form of high dispersion even atomic level dispersion, and the dispersion degree of the noble metal is 100 percent.
As can be seen from fig. 6: the catalyst has low dispersion degree of noble metal, and most of the noble metal is agglomerated together.
Claims (9)
1. The preparation method of the supported monatomic dispersed noble metal catalyst is characterized by comprising the following steps:
the preparation process comprises the following steps:
(1) dissolving a noble metal precursor in one or more than two solvents of deionized water or an organic solvent, and then adding one or more than two inorganic or organic reagents containing N, P, S to obtain a noble metal precursor complex solution;
(2) soaking a carrier into the noble metal precursor complex solution, stirring for 1-600 minutes, filtering, and drying at 60-120 ℃ for 6-12 hours to obtain a supported monoatomic dispersion noble metal catalyst precursor;
(3) placing the supported monoatomic noble metal catalyst precursor in a quartz tube, and adding He, Ar and N2、H2、O2Reducing at 200-800 deg.c for 10-600 sec in one or several kinds of air to obtain supported monoatomic dispersed noble metal catalyst; the carrier is one or more than two of oxide carrier or carbon material carrier;
the carrier oxide is one or a mixture of more than two of aluminum oxide, silicon oxide, ferric oxide, cerium oxide and titanium oxide in any ratio; the carrier carbon material is active carbon, acetylene black, mesoporous carbon material, graphene oxide, reduced graphene and C3N4One or a mixture of more than two of the above in any ratio.
2. A process for preparing a supported monatomic dispersed noble metal catalyst according to claim 1, wherein: the active component noble metal is one or mixture of more than two of ruthenium, rhodium, palladium, silver, iridium, platinum and gold in any ratio.
3. A process for the preparation of a supported monoatomic dispersion noble metal catalyst according to claim 1 or 2, wherein: based on the total weight of the catalyst, the content of the noble metal is 0.1 to 10 percent.
4. A process for the preparation of a supported monoatomic dispersion noble metal catalyst according to claim 1 or 2, wherein: the noble metal precursor is one or more of chloride, nitrate, acetylacetone complex and triphenylphosphine complex of noble metal.
5. A process for the preparation of a supported monatomic dispersed noble metal catalyst according to claim 1, characterized in that the organic solvent is: one or a mixture of more than two of methanol, ethanol, acetone, toluene, dichloromethane, tetrahydrofuran, n-hexane, isopropanol, DMF, DMSO, acetonitrile or other organic solvents in any ratio;
the inorganic reagent containing N, P, S comprises one or more than two of: one or a mixture of more than two of ammonia water, ammonium nitrate, ammonium chloride, ammonium carbonate, ammonium sulfate, ammonium sulfite, ammonium phosphate, ammonium phosphite or other N, P, S-containing inorganic reagents in any ratio; the N, P, S-containing organic reagent is one or more of ethylenediamine, diethylamine, ethanolamine, aniline, acetamide, EDTA, triphenylphosphine, triethyl phosphate, cystine, cysteine, or other organic reagent containing N, P, S, etc., at any ratio.
6. A process for preparing a supported monatomic dispersed noble metal catalyst according to claim 1, wherein: the mass concentration of the noble metal precursor in the step 1) is as follows: 0.0001 to 5 percent.
7. The process for preparing a supported monoatomic dispersion noble metal catalyst according to claim 1 or 6, wherein: the volume of the deionized water or the organic solvent is 5ml-50 ml; the mass of the added N, P, S-containing one or more inorganic or organic reagents is 0.0005g-10 g.
8. A process for preparing a supported monatomic dispersed noble metal catalyst according to claim 7, wherein: in order to ensure formation of the noble metal precursor complex solution, the ratio of the amount of one or more inorganic or organic reagents from N, P, S added to the amount of noble metal-containing substance added is 10:1 to 1000: 1.
9. A process for preparing a supported monatomic dispersed noble metal catalyst according to claim 1, wherein: the supported monoatomic dispersion noble metal catalyst prepared by the method consists of a carrier and an active component, wherein the active component is noble metal, the dispersion degree of the noble metal can reach atomic level dispersion, and the carrier is one or more than two of oxide or carbon materials; the dispersion of the noble metal is 100%.
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| CN111135840A (en) | 2020-05-12 |
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