CN108579761A - A kind of preparation method of the monatomic catalyst of the more metals of Pt-Ir/FeOx - Google Patents
A kind of preparation method of the monatomic catalyst of the more metals of Pt-Ir/FeOx Download PDFInfo
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- CN108579761A CN108579761A CN201810372017.8A CN201810372017A CN108579761A CN 108579761 A CN108579761 A CN 108579761A CN 201810372017 A CN201810372017 A CN 201810372017A CN 108579761 A CN108579761 A CN 108579761A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 93
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 44
- 239000002184 metal Substances 0.000 title claims abstract description 43
- 229910015189 FeOx Inorganic materials 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910002835 Pt–Ir Inorganic materials 0.000 title claims description 16
- 150000002739 metals Chemical class 0.000 title abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 47
- 239000012265 solid product Substances 0.000 claims abstract description 30
- 238000000975 co-precipitation Methods 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 230000008878 coupling Effects 0.000 claims abstract description 8
- 238000010168 coupling process Methods 0.000 claims abstract description 8
- 238000005859 coupling reaction Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 29
- 239000010453 quartz Substances 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 14
- 229910052741 iridium Inorganic materials 0.000 claims description 13
- 229910052697 platinum Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000012266 salt solution Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 37
- 230000003647 oxidation Effects 0.000 abstract description 26
- 230000003197 catalytic effect Effects 0.000 abstract description 11
- 239000006185 dispersion Substances 0.000 abstract description 4
- 239000003426 co-catalyst Substances 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 238000000034 method Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- 239000000446 fuel Substances 0.000 description 5
- 229910002621 H2PtCl6 Inorganic materials 0.000 description 4
- 238000004817 gas chromatography Methods 0.000 description 4
- 238000007493 shaping process Methods 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 238000006356 dehydrogenation reaction Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910002528 Cu-Pd Inorganic materials 0.000 description 1
- 229910017343 Fe2 (SO4)3 Inorganic materials 0.000 description 1
- 229910018054 Ni-Cu Inorganic materials 0.000 description 1
- 229910018481 Ni—Cu Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001651 catalytic steam reforming of methanol Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000007790 solid phase Substances 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
- B01J23/70—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
-
- 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
- B01J35/396—Distribution of the active metal ingredient
- B01J35/399—Distribution of the active metal ingredient homogeneously throughout the support particle
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
-
- 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
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses Pt Ir/FeOxThe preparation method of more monatomic catalyst of metal, includes the following steps：Step 1: microwave coupling coprecipitation reaction prepares catalyst；Step 2: washing and filtering solid product；Step 3: Pt Ir/FeO are made in drying and calcining solid productxMore monatomic catalyst of metal.The present invention is successfully prepared more metal polyatom catalyst on the basis of monometallic monatomic catalytic theory, realizes the monoatomic stable dispersion of more metals.Compared with general CO catalyst for selective oxidation, each metallic atom high degree of dispersion on carrier improves rate of metal, reduces cost.Compared with other are for the monatomic catalyst of CO selective oxidations, due to bimetallic synergistic effect, the load capacity and stability of monatomic catalyst are improved, there is higher catalytic activity.
Description
Technical field
The invention belongs to catalyst fields, are related to a kind of simultaneously in FeOxOn carrier in the form of monoatomic supporting Pt and Ir
Catalyst.
Background technology
Monatomic catalyst is a kind of new catalyst.It is structurally characterized in that is evenly distributed on carrier in the form of monoatomic
On.With nano-catalytic and sub-nanometer catalytic phase ratio, there are many new characteristics, as quantum size effect, huge surface are free
Energy, the interaction of carrier and metal and unsaturated coordination environment etc..Compared with nanocatalyst, on monatomic catalyst
Each atom is the activated centre of catalysis reaction, so greatly improving the selectivity of catalytic efficiency and reaction, and is reduced
Cost.
The preparation method of monatomic catalyst has coprecipitation, atom deposition method, infusion process, gradually reduction method, anti-
Ostwald cures method, gradually reduction method and solid phase fusion method.
Coprecipitation refers to containing 2 kinds or cation of more than two kinds in solution, their equal distributed mutuallies in the solution are added
After precipitating reagent, the uniform precipitation of various composition can be obtained.
Current monatomic catalyst has been used for CO oxidations, hydrogenation, NO reduction and hydrogenation, Water gas shift/WGS, You Jihe
At, methanol steam reforming, fuel cell, photoelectrocatalysis, oxidation of formaldehyde etc..But monatomic catalyst is due to its huge surface
Free energy is easily coupled into huge cluster, and then leads to catalyst inactivation in the preparation.And in order to prevent this situation, single
Load capacity on catalyst atom is often very low, and which has limited the practical applications of monatomic catalyst.
Current monatomic catalyst all only has a kind of metal to be supported on carrier in the form of monoatomic.It is general mostly golden
Metal catalyst, compared with pure metal catalyst, stability greatly improves.Such as the Pt-Ir catalysis that in the oil industry, light oil is reformed
The stability of agent is greatly improved than the stability of pure Pt.Therefore the monatomic catalyst of more metals is developed, it is possible to enhance catalyst
Stability, improve load capacity.
In addition, general multimetal reforming catalyst compared with pure metal catalyst, has higher reactivity, selectivity.
Cost can also be reduced.If the pure Ni of the reactivity ratio of Pd-Ni catalyst is good, in selective hydrogenation of acetylene reaction, Cu-Pd is urged
The activity of agent is not only better than Pd, but also since Pd is a kind of rare noble metal, expensive, and Cu, which is added, to be reduced into
This, therefore the monatomic catalyst of more metals is possible to also have these excellent performances, in the conversion of hexamethylene, Ni catalyst
Benzene can be produced in dehydrogenation reaction, also have by-product production methane etc..And it will greatly improve dehydrogenation using Ni-Cu catalyst and select
Selecting property.In addition, some catalysis reactions need various metals to coordinate catalysis.The preparation of more monatomic catalyst of metal will be so that single former
The research range of muonic catalysis agent is expanded significantly.
Hydrogen in fuel cell often contains 0.5% to 2% CO, since the anode electrocatalyst of fuel cell is usually
Pt, CO are easily adsorbed in the surface of catalyst, and then obstruct the catalysis oxidation of fuel, as long as research shows that having micro CO can
To cause Pt anode catalysts to be inactivated because CO is poisoned.Cause fuel cell that can not use.The CO of chemical method removal at present is main
There are anode note oxygen, low temperature shift reaction method, methanation reaction method, selective catalytic oxidation method.Wherein selective catalytic oxidation method
It is most efficient method.Using metals such as Pt, Ru, Pd as catalyst when selective catalytic oxidation method, selective oxidation hydrogen-rich gas
In CO.
Xiao Gang etc. is prepared for the integral catalyzer (patent No. of CO in selective oxidation hydrogen-rich reformed gas a kind of：
ZL200810301388.3), the catalytic active component of the patent is Ru, and content is 0.1-2wt% in terms of Ru；Catalyst aid is alkali
One or more of metal oxide or/and alkaline earth oxide；Ru and alkali metal oxide or/and alkali metal oxide
The molar ratio of middle metallic element is 1-20: 1；Remaining is the cordierite carrier for applying aluminium glue, and the content of wherein aluminium glue accounts for catalyst
Content is 2-10wt%.Complicated, price is high, and reactivity is relatively low.
Invention content
It is an object of the invention to overcome the deficiencies of the prior art and provide one kind with FeOxIt, can be simultaneously with single original for carrier
The monatomic catalyst of sub- form supporting Pt and Ir, to improve the content of metal of catalyst, the Pt- of catalytic activity and selectivity
The preparation method of the monatomic catalyst of the more metals of Ir/FeOx.
The present invention relates to Pt-Ir/FeOxThe preparation method of more monatomic catalyst of metal, includes the following steps：
Step 1: microwave coupling coprecipitation reaction prepares catalyst, the specific steps are：
By the H of isometric a concentration of 0.02-1.2mol/L2PtCl6Solution, a concentration of 0.02-1.2mol/L
H2IrCl6Solution is mixed with water-soluble ferric salt solution of a concentration of 1mol/L, then by the alkalinity of a concentration of 1mol/L
Substance solution is added to mixed solution, adjusts the pH to 8 of mixed solution, coprecipitation reaction is carried out at 20 DEG C -80 DEG C, then will
Acquired solution is put into microwave reactor and heats, and makes catalyst Pt and Ir at carrier Fe (OH)3On be evenly distributed；
Step 2: washing and filtering solid product, the specific steps are：
Solid product obtained is washed with distilled water, is then filtered with vacuum pump, it is remaining in solid product to remove
Ion；
Step 3: drying and calcining solid product, the specific steps are：
It is placed in the product after filtering and washing is evenly laid out in microwave dryer and dries on quartz plate, go
Moisture removal, the material thickness being laid on quartz plate are less than 2mm, then calcine the product of drying 4-5 hours at 400 DEG C,
Carrier Fe (OH) in this way3It is converted into FeOx, Pt-Ir/FeO is madexMore monatomic catalyst of metal.
The beneficial effects of the invention are as follows：
The present invention is successfully prepared more metal polyatom catalyst on the basis of monometallic monatomic catalytic theory, real
The monoatomic stable dispersion of more metals is showed.Compared with general CO catalyst for selective oxidation, each metallic atom is in carrier
Upper high degree of dispersion, improves rate of metal, reduces cost.The monatomic catalyst phase of CO selective oxidations is used for other
Than due to bimetallic synergistic effect, improving the load capacity and stability of monatomic catalyst, there is higher catalysis to live
Property.
Description of the drawings
Fig. 1 is that CO is aoxidized in example 1 and the reaction rate of CO preferential oxidations is with coprecipitation reaction temperature in catalyst preparation
The relational graph of variation.
Specific implementation mode
With reference to specific example, the present invention is described in detail
The present invention relates to Pt-Ir/FeOxThe preparation method of more monatomic catalyst of metal, includes the following steps：
Step 1: microwave coupling coprecipitation reaction prepares catalyst, the specific steps are：
By the H of isometric a concentration of 0.02-1.2mol/L2PtCl6Solution, a concentration of 0.02-1.2mol/L
H2IrCl6Solution is mixed with the water-soluble ferric salt solutions of a concentration of 1mol/L, then by the basic species of a concentration of 1mol/L
Matter solution is added to mixed solution, adjusts the pH to 8 of mixed solution, and it is (preferred total that coprecipitation reaction is carried out at 20 DEG C -80 DEG C
Precipitation reaction 8-24 hours).Then acquired solution is put into microwave reactor and is heated 2-10 minutes at 100-200 DEG C,
Make catalyst Pt and Ir at carrier Fe (OH)3On be evenly distributed.Reaction temperature is not under conditions of influencing coprecipitation reaction progress
It chooses.The trivalent iron salt is not limited to Fe (NO3)3, contain Fe3+Molysite, may serve to prepare catalyst；Alkaline matter is simultaneously
It is not limited to Na2CO3, all alkaline matters for adjusting pH.
Step 2: washing and filtering solid product, the specific steps are：
Solid product obtained is washed with distilled water, is then filtered with vacuum pump, it is remaining in solid product to remove
Ion.
Step 3: drying and calcining solid product, the specific steps are：
It is placed in the product after filtering and washing is evenly laid out in microwave dryer and dries on quartz plate, go
Moisture removal, the material thickness being laid on quartz plate are less than 2mm, then calcine the product of drying 4-5 hours at 400 DEG C,
Obtain Pt-Ir/FeOxMore monatomic catalyst of metal.
The vacuum pump can be replaced with other filtering apparatus.
Embodiment 1
Step 1: microwave coupling coprecipitation reaction prepares catalyst
By 500ml H2PtCl6(0.06mol/L)、500ml H2IrCl6(0.02mol/L) solution and 500ml Fe (NO3)3
(1mol/L) is mixed, and passes through Na2CO3(1mol/L) adjusts solution PH to 8, coprecipitation reaction is carried out at 20 DEG C 8 hours.Then
Acquired solution is put into microwave reactor be heated to 100 DEG C react 2 minutes, make catalyst Pt and Ir at carrier Fe (OH)3On
It is evenly distributed.
Step 2: the washing and filtering of solid product
Solid product obtained is washed with distilled water, is then filtered with vacuum pump, it is remaining in solid product to remove
Ion.
Step 3: the drying and calcining of solid product
By the product after filtering and washing it is evenly laid out on quartz plate, be placed in microwave dryer dry removal
Moisture, the material thickness 1.9mm being laid on quartz plate then calcine the product of drying 4 hours, carrier Fe at 400 DEG C
(OH)3It is converted into FeOx, Pt-Ir/FeO is madexMore monatomic catalyst of metal.
To the Pt-Ir/FeO of preparationxThe activity and selectivity of more monatomic catalyst of metal is evaluated, the specific steps are：
CO oxidation reactions：It is reacted by the oxidation of the CO in fixed bed and the preferential oxidation of CO to measure the reaction of catalyst
Activity.It is first granular by shaping of catalyst, the catalyst for then weighing 80mg or so is put into U-shaped quartz reactor, is in temperature
Be passed through under conditions of 200 DEG C volume ratio be 10% He pre-process 0.5 hour after, test is passed through with the speed of 25ml per minute
Gas, test gas volume fractions are respectively CO1%, O21%, He are Balance Air.It is online with gas-chromatography and thermal conductivity detector (TCD)
Detect the gas componant of discharge.
The preferential oxidation reaction of CO is similar therewith, in the test gas being passed through, H240%, CO1%, O21%, He are balance
Gas, other steps are identical.
The result shows that the catalyst Pt load capacity prepared is 0.15wt%, Ir load capacity is 0.04wt%, anti-in CO oxidations
Ying Zhong, reaction rate 6020molco h-1gmetal -1, in the reaction of CO preferential oxidations, reaction rate 9930molco h- 1gmetal -1.Selectivity is 50%.Fig. 1 is the pass between the temperature of coprecipitation reaction and catalyst reaction activity in catalyst preparation
System, it can be seen that with temperature rise, the catalytic activity and selectivity of catalyst both increase.
Embodiment 2
Step 1: microwave coupling coprecipitation reaction prepares catalyst
By 500ml H2PtCl6(0.02mol/L)、500ml H2IrCl6(0.06mol/L) solution and 500ml Fe2
(SO4)3(1mol/L) is mixed, and passes through Na2CO3(1mol/L) adjusts solution PH to 8, and it is small that coprecipitation reaction 11 is carried out at 80 DEG C
When.Then acquired solution is put into microwave reactor be heated to 200 DEG C react 2 minutes, make catalyst Pt and Ir in carrier Fe
(OH)3On be evenly distributed.
Step 2: the washing and filtering of solid product
Solid product obtained is washed with distilled water, is then filtered with vacuum pump, it is remaining in solid product to remove
Ion.
Step 3: the drying and calcining of solid product
By the product after filtering and washing it is evenly laid out on quartz plate, be placed in microwave dryer dry removal
Moisture, the material thickness being laid on quartz plate is 1.8mm, then calcines the product of drying 4.5 hours at 400 DEG C, is carried
Body Fe (OH)3It is converted into FeOx, Pt-Ir/FeO is madexMore monatomic catalyst of metal.
The activity and selectivity of catalyst is evaluated, the specific steps are：
CO oxidation reactions：It is reacted by the oxidation of the CO in fixed bed and the preferential oxidation of CO to measure the reaction of catalyst
Activity.It is first granular by shaping of catalyst, the catalyst for then weighing 80mg or so is put into U-shaped quartz reactor, is in temperature
It is passed through H under conditions of 200 DEG C2After the He that volume ratio is 10% is pre-processed 0.5 hour, survey is passed through with the speed of 25ml per minute
Gas testing body, test gas volume fractions are respectively CO1%, O21%, He are Balance Air.Existed with gas-chromatography and thermal conductivity detector (TCD)
The gas componant of line detection discharge.
The preferential oxidation reaction of CO is similar therewith, in the test gas being passed through, H240%, CO1%, O21%, He are balance
Gas, other steps are identical.
The result shows that the catalyst Pt load capacity prepared is 0.04wt%, Ir load capacity is 1.5wt%, in CO oxidation reactions
In, reaction rate 6520molco h-1gmetal -1, in the reaction of CO preferential oxidations, reaction rate 8720molco h-1gmetal -1.Selectivity is 50%.
Embodiment 3
Step 1: microwave coupling coprecipitation reaction prepares catalyst
By 500ml H2PtCl6(0.2mol/L)、500ml H2IrCl6(1.2mol/L) solution and Fe (NO)3(1mol/L)
Solution mixes, and adjusts pH value of solution to 8 by NaOH (1mol/L), coprecipitation reaction is carried out at 80 DEG C 16 hours.Then by institute
Solution be put into microwave reactor be heated to 170 DEG C react 5 minutes, make catalyst Pt and Ir at carrier Fe (OH)3Upper distribution
Uniformly.
Step 2: the washing and filtering of solid product
Solid product obtained is washed with distilled water, is then filtered with vacuum pump, it is remaining in solid product to remove
Ion.
Step 3: the drying and calcining of solid product
By the product after filtering and washing it is evenly laid out on quartz plate, be placed in microwave dryer dry removal
Moisture, the material thickness being laid on quartz plate is 1mm, is then calcined the product of drying 5 hours at 400 DEG C, carrier Fe
(OH)3It is converted into FeOx, Pt-Ir/FeO is madexMore monatomic catalyst of metal.
The activity and selectivity of catalyst is evaluated, the specific steps are：
CO oxidation reactions：It is reacted by the oxidation of the CO in fixed bed and the preferential oxidation of CO to measure the reaction of catalyst
Activity.It is first granular by shaping of catalyst, the catalyst for then weighing 80mg or so is put into U-shaped quartz reactor, is in temperature
It is passed through H under conditions of 200 DEG C2After the He that volume ratio is 10% is pre-processed 0.5 hour, survey is passed through with the speed of 25ml per minute
Gas testing body, test gas volume fractions are respectively CO1%, O21%, He are Balance Air.Existed with gas-chromatography and thermal conductivity detector (TCD)
The gas componant of line detection discharge.
The preferential oxidation reaction of CO is similar therewith, in the test gas being passed through, H240%, CO1%, O21%, He are balance
Gas, other steps are identical.
The result shows that the catalyst Pt load capacity prepared is 0.41wt%, Ir load capacity is 3.0wt%, in CO oxidation reactions
In, reaction rate 81230molco h-1gmetal -1, in the reaction of CO preferential oxidations, reaction rate 163920molco h- 1gmetal -1.Selectivity is 56%.
Embodiment 4
Step 1: microwave coupling coprecipitation reaction prepares catalyst
By 500ml H2PtCl6(1.2mol/L)、500ml H2IrCl6(0.4mol/L) solution and 500ml Fe (NO)3
(1mol/L) solution mixes, and passes through Na2CO3(1mol/L) adjusts solution PH to 8, coprecipitation reaction is carried out at 60 DEG C 24 hours.
Then acquired solution is put into microwave reactor be heated to 200 DEG C react 10 minutes, make catalyst Pt and Ir in carrier Fe
(OH)3On be evenly distributed.
Step 2: the washing and filtering of solid product
Solid product obtained is washed with distilled water, is then filtered with vacuum pump, it is remaining in solid product to remove
Ion.
Step 3: the drying and calcining of solid product
By the product after filtering and washing it is evenly laid out on quartz plate, be placed in microwave dryer dry removal
Moisture, the material thickness being laid on quartz plate is 0.5mm, is then calcined the product of drying 5 hours at 400 DEG C, carrier
Fe(OH)3It is converted into FeOx, Pt-Ir/FeO is madexMore monatomic catalyst of metal.
The activity and selectivity of catalyst is evaluated, the specific steps are：
CO oxidation reactions：It is reacted by the oxidation of the CO in fixed bed and the preferential oxidation of CO to measure the reaction of catalyst
Activity.It is first granular by shaping of catalyst, the catalyst for then weighing 80mg or so is put into U-shaped quartz reactor, is in temperature
It is passed through H under conditions of 200 DEG C2After the He that volume ratio is 10% is pre-processed 0.5 hour, survey is passed through with the speed of 25ml per minute
Gas testing body, test gas volume fractions are respectively CO1%, O21%, He are Balance Air.Existed with gas-chromatography and thermal conductivity detector (TCD)
The gas componant of line detection discharge.
The preferential oxidation reaction of CO is similar therewith, in the test gas being passed through, H240%, CO1%, O21%, He are balance
Gas, other steps are identical.
The result shows that the catalyst Pt load capacity prepared is 3.1wt%, Ir load capacity is 0.81wt%, in CO oxidation reactions
In, reaction rate 99830molco h-1gmetal -1, in the reaction of CO preferential oxidations, reaction rate 198320molco h- 1gmetal -1.Selectivity is 56%.
Claims (3)
1. a kind of Pt-Ir/FeOxThe preparation method of more monatomic catalyst of metal, it is characterised in that include the following steps：
Step 1: microwave coupling coprecipitation reaction prepares catalyst, the specific steps are：
By the H of isometric a concentration of 0.02-1.2mol/L2PtCl6The H of solution, a concentration of 0.02-1.2mol/L2IrCl6Solution
It mixes with water-soluble ferric salt solution of a concentration of 1mol/L, then adds the alkaline substance solution of a concentration of 1mol/L
Enter to mixed solution, adjusts the pH to 8 of mixed solution, coprecipitation reaction is carried out at 20 DEG C -80 DEG C, then puts acquired solution
Enter in microwave reactor and heat, makes catalyst Pt and Ir at carrier Fe (OH)3On be evenly distributed；
Step 2: washing and filtering solid product, the specific steps are：
Solid product obtained is washed with distilled water, is then filtered with vacuum pump, to remove remaining ion in solid product；
Step 3: drying and calcining solid product, the specific steps are：
It is placed in the product after filtering and washing is evenly laid out in microwave dryer and dries on quartz plate, go to remove water
Point, it is laid in material thickness on quartz plate and is less than 2mm, the product of drying then calcined to 4-5 hours at 400 DEG C, in this way
Carrier Fe (OH)3It is converted into FeOx, Pt-Ir/FeO is madexMore monatomic catalyst of metal.
2. Pt-Ir/FeO according to claim 1xThe preparation method of more monatomic catalyst of metal, it is characterised in that：Institute
The coprecipitation reaction stated 8-24 hours.
3. Pt-Ir/FeO according to claim 1 or 2xThe preparation method of more monatomic catalyst of metal, feature exist
In：Solution is put into microwave reactor after coprecipitation reaction heats 2-10 minutes at 100-200 DEG C.
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