CN105457629A - Load type nano precious metal catalyst and preparation method and application thereof - Google Patents
Load type nano precious metal catalyst and preparation method and application thereof Download PDFInfo
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- CN105457629A CN105457629A CN201510925106.7A CN201510925106A CN105457629A CN 105457629 A CN105457629 A CN 105457629A CN 201510925106 A CN201510925106 A CN 201510925106A CN 105457629 A CN105457629 A CN 105457629A
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- precious metal
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- 239000003054 catalyst Substances 0.000 title claims abstract description 73
- 239000010970 precious metal Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000011148 porous material Substances 0.000 claims abstract description 10
- 229910000510 noble metal Inorganic materials 0.000 claims description 62
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 18
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 18
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 239000010931 gold Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000002923 metal particle Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 11
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 239000000446 fuel Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 2
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 238000002407 reforming Methods 0.000 claims description 2
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 23
- 239000000084 colloidal system Substances 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 5
- 239000000969 carrier Substances 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 101150003085 Pdcl gene Proteins 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000001802 infusion Methods 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
- B01J23/44—Palladium
-
- 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
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- 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
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- 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
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
-
- B01J35/23—
-
- B01J35/393—
-
- B01J35/613—
-
- B01J35/615—
-
- B01J35/633—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/12—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents by reaction of water vapour with carbon monoxide
- C01B3/16—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents by reaction of water vapour with carbon monoxide using catalysts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
- C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
- C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
- C01B3/40—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts characterised by the catalyst
-
- 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
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
- C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
- C01B2203/0233—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step the reforming step being a steam reforming step
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a load type nano precious metal catalyst which comprises a carrier and nano precious metal particles loaded on the carrier. The average particle size of the nano precious metal particles is 1.5-4.5 nm, and the quality percentage of the precious metal in the catalyst is 1-10%; the specific surface area of the carrier is 40-190 m<2>/g, and the pore volume is 0.06-0.4 ml/g. The preparation method of the catalyst includes the steps that a reduction method is adopted to prepare nano precious metal colloid particles, then a colloidal deposition method is adopted, the nano precious metal particles are loaded to different carriers, and the load type nano precious metal catalyst with the particle size and the size distribution being the same is prepared. The load type nano precious metal catalyst can be widely applied to an industrial catalytic reaction, and the emission load of the pollutant CO can be lowered.
Description
Technical field
The present invention relates to nanocatalyst preparing technical field, be specifically related to a kind of loaded nano noble metal catalyst and its preparation method and application.
Background technology
Nano particle makes to which create much distinctive optics, electricity, catalytic performance etc. because of the quantum size effect of its uniqueness, skin effect and macro quanta tunnel effect etc., the fields such as chemical industry, electronic circuit, optical check, instrument manufacturing, bio-sensing, pharmaceutical carrier can be widely used in, there is important using value.
Air pollution problems inherent more and more receives the concern of people, and many researchers start to be devoted to research and develop efficient, safe, economic material for air purification.Wherein the efficient performance of loaded nano noble metal granule causes the attention of researcher.Nano-noble metal particle because of its valuable rare characteristic, can not individually, a large amount of stable existence, be therefore loaded on cheap inert carrier, generate loaded nano noble metal catalyst and catalytic action is carried out to industrial reaction.
The method of loaded nano noble metal catalyst is generally infusion process, deposition-precipitation etc.In these conventional methods, even if preparation condition (as pH value, aging, roasting etc.) is identical, but due to the difference of oxide carrier kind, also can impact the formation of nano metal particles, make the size of nano noble metal particles and Size Distribution different and produce larger difference.Wherein on loaded nano noble metal catalyst, nano particle plays catalytic effect, and because the particle diameter of nano noble metal particles is different, its performance can be greatly affected, and therefore the loaded nano noble metal catalyst prepared of conventional method is unsatisfactory.
Summary of the invention
In order to overcome prior art deficiency, the invention provides a kind of loaded nano noble metal catalyst and its preparation method and application.Preparation method of the present invention first adopts reducing process to prepare nano-noble metal colloidal particle, then by colloidal deposition method, nano noble metal particles is loaded on different carriers, prepares grain size and the identical loaded nano noble metal catalyst of Size Distribution.
Technical solution of the present invention is as follows:
A kind of loaded nano noble metal catalyst, comprise carrier and be carried on the nano-noble metal particle on described carrier, the average grain diameter of wherein said nano-noble metal particle is 1.5-4.5nm, and in catalyst, the mass percentage of noble metal is 1%-10%; The specific area of described carrier is 40-190m
2/ g, pore volume is 0.06-0.4ml/g.
Preferably, the average grain diameter of described nano-noble metal particle is 1.5-3nm, more preferably 2nm;
Preferably, in described catalyst, the mass percentage of noble metal is 1%-1.5%, more preferably 1%;
Preferably, the specific area of described carrier is specific area is 40-60m
2/ g, pore volume is 0.06-0.1ml/g.
Preferably, described noble metal comprises one or more in Pt, Pd, Au, Rh, Ag, Ru etc.; More preferably Pt and/or Au.
Preferably, described carrier is TiO
2, CeO
2, ZrO
2, Al
2o
3deng one or more in oxide; More preferably TiO
2and/or CeO
2.
The present invention also provides the preparation method of above-mentioned loaded nano noble metal catalyst, comprises the steps:
1) be dissolved in by precious metal salt in PVP (i.e. polyvinylpyrrolidone) solution, add the ethylene glycol solution containing NaOH, continue to pass into inert gas, after stirring, cooling, obtains the nano-sized colloidal solution of described noble metal;
2) add acid to receiving in colloidal solution of described noble metal, add inert carrier after centrifugation, after leaving standstill, dry process, obtains loaded nano noble metal catalyst.
The preparation method of above-mentioned loaded nano noble metal catalyst, wherein:
Step 1) described precious metal salt comprises chloroplatinic acid (H
2ptCl
66H
2o), gold chloride (HAuCl
44H
2o), palladium bichloride (PdCl
2nH
2o), ruthenium trichloride (RuCl
3nH
2etc. O) one or more in;
Described polyvinylpyrrolidonesolution solution concentration is 1 × 10
-6-1 × 10
-5mol/L;
The concentration of described precious metal salt in polyvinylpyrrolidonesolution solution is 0.003-0.03mmol/L, is preferably 0.025-0.029mmol/L;
The concentration of described NaOH in ethylene glycol is 0.02-0.05mmol/L, is preferably 0.02-0.03mmol/L;
Described inert gas is one or more in argon gas, nitrogen, helium etc.;
Step 2) described acid is one or more in hydrochloric acid, nitric acid, carbonic acid etc.; Be preferably hydrochloric acid.
The consumption of described acid is 0.02-0.03mmol/L;
Described inert carrier comprises TiO
2, CeO
2, ZrO
2, Al
2o
3deng one or more in oxide; More preferably TiO
2and/or CeO
2.
The present invention also comprises the obtained loaded nano noble metal catalyst of said method.
The present invention also provides the purposes of above-mentioned loaded nano noble metal catalyst, and described purposes comprises for hydrogen manufacturing, methane vapor reforming legal system synthesis gas etc. in hydrogen/methanol oxidation in fuel cell or redox, water gas shift reaction.
If no special instructions, specific area method of testing of the present invention is static capacity method.
The present invention obtains grain size and the identical nano-noble metal particle of Size Distribution by reducing process, then loads on different inert carriers, obtains the catalyst that nano-noble metal seed activity is identical.Method is reduced the nano-noble metal grain diameter obtained and is about 2nm thus, and domain size distribution is more even.By nano-noble metal particulate load on identical indifferent oxide carrier, obtained loaded nano noble metal catalyst, can be widely used in industrial catalytic reaction.Loaded nano noble metal catalyst involved in the present invention, can be applicable in small-sized even medium-sized fuel cell, reduces the discharge capacity of pollutant CO.
Accompanying drawing explanation
Fig. 1 is embodiment 1Pt/TiO
2tEM figure (i.e. transmission electron microscope picture) of catalyst.
Fig. 2 is different preparation method Pt/CeO in experimental example 1
2catalyst carries out the CO conversion ratio figure of water gas shift reaction.
Detailed description of the invention
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
If no special instructions, specific area method of testing described in following examples is static capacity method.
Embodiment 1
A kind of loaded nano precious metals pt catalyst (Pt/TiO
2catalyst), nano-noble metal Pt particle diameter is 2nm, and carrier is TiO
2, the specific area of this carrier is 40m
2/ g, pore volume is 0.06ml/g, and in catalyst, the mass percentage of precious metals pt is 1%.
Embodiment 2
A kind of loaded nano precious metals pt catalyst (Pt/CeO
2catalyst), nano-noble metal Pt particle diameter is 2nm, and carrier is CeO
2, the specific area of this carrier is 60m
2/ g, pore volume is 0.1ml/g, and in catalyst, the mass percentage of precious metals pt is 1%.
Embodiment 3
A kind of loaded nano noble metal Au catalyst (Au/TiO
2catalyst), nano-noble metal Au particle diameter is 2nm, and carrier is TiO
2, the specific area of this carrier is 40m
2/ g, pore volume is 0.06ml/g, and in catalyst, the mass percentage of noble metal Au is 1%.
Embodiment 4
A kind of loaded nano precious metals pd catalyst (Pd/TiO
2catalyst), nano-noble metal Pd particle diameter is 2nm, and carrier is TiO
2, the specific area of this carrier is 40m
2/ g, pore volume is 0.06ml/g, and in catalyst, the mass percentage of precious metals pd is 1%.
Embodiment 5
A kind of loaded nano precious metals pd catalyst (Pd/CeO
2catalyst), nano-noble metal Pd particle diameter is 2nm, and carrier is CeO
2, the specific area of this carrier is 60m
2/ g, pore volume is 0.1ml/g, and in catalyst, the mass percentage of precious metals pd is 1%.
Embodiment 6
The present embodiment provides loaded nano precious metals pt catalyst (Pt/TiO described in embodiment 1
2catalyst) preparation method, comprise the following steps:
By a certain amount of H
2ptCl
66H
2o solid is dissolved in PVP solution that (PVP solution concentration is 1 × 10
-5mol/L), add the ethylene glycol solution containing NaOH, after mixing, be placed in three hole round-bottomed flasks, described H
2ptCl
66H
2the concentration of O in PVP solution is 0.029mmol/L; The concentration of described NaOH in ethylene glycol is 0.02mmol/L; Continue to pass into inert gas argon gas, after stirring, cooling obtains the nano-colloid particle solution of precious metals pt.This nano-colloid particle solution is added the HCl of 0.02mmol/L amount, after centrifugation, add inert carrier TiO
2, stir, carry out drying process after leaving standstill, obtain loaded nano precious metals pt catalyst.
Embodiment 7
The present embodiment provides loaded nano precious metals pt catalyst (Pt/CeO described in embodiment 2
2catalyst) preparation method, comprise the following steps:
By a certain amount of H
2ptCl
66H
2o solid is dissolved in PVP solution that (PVP solution concentration is 1 × 10
-5mol/L), add the ethylene glycol solution containing NaOH, after mixing, be placed in three hole round-bottomed flasks, described H
2ptCl
66H
2the concentration of O in PVP solution is 0.029mmol/L; The concentration of described NaOH in ethylene glycol is 0.02mmol/L; Continue to pass into inert gas argon gas, after stirring, cooling obtains the nano-colloid particle solution of precious metals pt.This nano-colloid particle solution is added the HCl of 0.02mmol/L amount, after centrifugation, add inert carrier CeO
2, stir, carry out drying process after leaving standstill, obtain loaded nano precious metals pt catalyst.
Embodiment 8
The present embodiment provides loaded nano noble metal Au catalyst (Au/TiO described in embodiment 3
2catalyst) preparation method, comprise the following steps:
By a certain amount of HAuCl
44H
2o solid is dissolved in PVP solution that (PVP solution concentration is 1 × 10
-6mol/L), add the ethylene glycol solution containing NaOH, after mixing, be placed in three hole round-bottomed flasks, described HAuCl
44H
2the concentration of O in PVP solution is 0.03mmol/L; The concentration of described NaOH in ethylene glycol is 0.02mmol/L; Continue to pass into inert nitrogen gas, after stirring, cooling obtains the nano-colloid particle solution of noble metal Au.This nano-colloid particle solution is added the HCl of 0.02mmol/L amount, after centrifugation, add inert carrier TiO
2, stir, carry out drying process after leaving standstill, obtain loaded nano precious metals pt catalyst.
Embodiment 9
The present embodiment provides loaded nano precious metals pd catalyst (Pd/TiO described in embodiment 4
2catalyst) preparation method, comprise the following steps:
By a certain amount of PdCl
2nH
2o solid is dissolved in PVP solution that (PVP solution concentration is 1 × 10
-6mol/L), add hydrochloric ethylene glycol solution, after mixing, be placed in three hole round-bottomed flasks, described PdCl
2nH
2the concentration of O in PVP solution is 0.03mmol/L; The concentration of described NaOH in ethylene glycol is 0.02mmol/L; Continue to pass into inert nitrogen gas, after stirring, cooling obtains the nano-colloid particle solution of noble metal Au.This nano-colloid particle solution is added the NaOH of 0.02mmol/L amount, after centrifugation, add inert carrier TiO
2, stir, carry out drying process after leaving standstill, obtain loaded nano precious metals pt catalyst.
Embodiment 10
The present embodiment provides loaded nano noble metal Au catalyst (Au/TiO described in embodiment 3
2catalyst) preparation method, comprise the following steps:
By a certain amount of HAuCl
44H
2o solid is dissolved in PVP solution that (PVP solution concentration is 1 × 10
-5mol/L), add the ethylene glycol solution containing NaOH, after mixing, be placed in three hole round-bottomed flasks, described HAuCl
44H
2the concentration of O in PVP solution is 0.03mmol/L; The concentration of described NaOH in ethylene glycol is 0.02mmol/L; Continue to pass into inert nitrogen gas, after stirring, cooling obtains the nano-colloid particle solution of noble metal Au.This nano-colloid particle solution is added the HCl of 0.02mmol/L amount, after centrifugation, add inert carrier CeO
2, stir, carry out drying process after leaving standstill, obtain loaded nano precious metals pt catalyst.
Comparative example 1
A kind of loaded nano precious metals pt catalyst (Pt/CeO
2catalyst), by prior art loaded catalyst conventional impregnation methods, by carrier (CeO
2) put liquid (H containing active material into
2ptCl
6solution) middle dipping, active material (Pt ion) is adsorbed in carrier surface gradually, and when after dipping balance, the liquid that removing is left, carries out the process such as drying, roasting and prepare.
Experimental example 1
Adopt Pt/CeO described in embodiment 1 and comparative example 1 respectively
2catalyst carries out Water gas shift/WGS (CO+H
2o=CO
2+ H
2) reaction, result (as shown in Figure 2) shows, CO conversion ratio raises with the rising of temperature, under same temperature, catalyst described in the embodiment of the present invention 1 in the reaction CO conversion ratio apparently higher than the catalyst prepared by conventional infusion process (comparative example 1).In Fig. 2, abscissa represents temperature, and ordinate represents CO conversion ratio, and " Xeqco " represents the thermodynamical equilibrium conversion ratio of water gas shift reaction, " Pt/CeO
2infusion process " represent comparative example 1, " Pt/CeO
2method therefor of the present invention " represent embodiment 1.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (10)
1. a loaded nano noble metal catalyst, comprise carrier and be carried on the nano-noble metal particle on described carrier, the average grain diameter of wherein said nano-noble metal particle is 1.5-4.5nm, and in catalyst, the mass percentage of noble metal is 1%-10%; The specific area of described carrier is 40-190m
2/ g, pore volume is 0.06-0.4ml/g.
2. loaded nano noble metal catalyst according to claim 1, is characterized in that, the average grain diameter of described nano-noble metal particle is 1.5-3nm, is preferably 2nm;
Preferably, in described catalyst, the mass percentage of noble metal is 1%-1.5%, more preferably 1%;
Preferably, the specific area of described carrier is 40-60m
2/ g, pore volume is 0.06-0.1ml/g.
3. loaded nano noble metal catalyst according to claim 1 and 2, is characterized in that, described noble metal comprises one or more in Pt, Pd, Au, Rh, Ag, Ru; Be preferably Pt and/or Au.
4. loaded nano noble metal catalyst according to claim 1 and 2, is characterized in that, described carrier is TiO
2, CeO
2, ZrO
2, Al
2o
3in one or more; Be preferably TiO
2and/or CeO
2.
5. the preparation method of loaded nano noble metal catalyst described in any one of claim 1-4, is characterized in that, comprise the steps:
1) be dissolved in polyvinylpyrrolidonesolution solution by precious metal salt, add the ethylene glycol solution containing NaOH, continue to pass into inert gas, after stirring, cooling, obtains the nano-sized colloidal solution of described noble metal;
2) add acid to receiving in colloidal solution of described noble metal, add inert carrier after centrifugation, after leaving standstill, dry process, obtains loaded nano noble metal catalyst.
6. preparation method according to claim 5, is characterized in that, step 1) described in precious metal salt comprise in chloroplatinic acid, gold chloride, palladium bichloride, ruthenium trichloride one or more;
Preferably, the concentration of described precious metal salt in polyvinylpyrrolidone is 0.003-0.03mmol/L, more preferably 0.025-0.029mmol/L;
Preferably, described polyvinylpyrrolidonesolution solution concentration is 1 × 10-6-1 × 10-5mol/L.
7. the preparation method according to claim 5 or 6, is characterized in that, step 1) described in the concentration of NaOH in ethylene glycol be 0.02-0.05mmol/L, be preferably 0.02-0.03mmol/L;
Preferably, inert gas is one or more in argon gas, nitrogen, helium.
8. the preparation method according to any one of claim 5-7, is characterized in that, step 2) described in acid be one or more in hydrochloric acid, nitric acid, carbonic acid; Be preferably hydrochloric acid; Preferably, the consumption of described acid is 0.02-0.03mmol/L.
9. the preparation method according to any one of claim 5-8, is characterized in that, step 2) described in inert carrier comprise in TiO2, CeO2, ZrO2, Al2O3 one or more; Be preferably TiO2 and/or CeO2.
10. the purposes of loaded nano noble metal catalyst prepared by method described in the loaded nano noble metal catalyst described in any one of claim 1-4 or any one of claim 5-9, described purposes comprises for hydrogen manufacturing in hydrogen/methanol oxidation in fuel cell or oxygen reduction, water gas shift reaction, methane vapor reforming method preparing synthetic gas.
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