CN106582638B - A kind of (Au, Rh)-Ce applied to NO+CO reactionx/Al2O3Preparation method - Google Patents
A kind of (Au, Rh)-Ce applied to NO+CO reactionx/Al2O3Preparation method Download PDFInfo
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- CN106582638B CN106582638B CN201611226042.2A CN201611226042A CN106582638B CN 106582638 B CN106582638 B CN 106582638B CN 201611226042 A CN201611226042 A CN 201611226042A CN 106582638 B CN106582638 B CN 106582638B
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8643—Removing mixtures of carbon monoxide or hydrocarbons and nitrogen oxides
- B01D53/8646—Simultaneous elimination of the components
- B01D53/865—Simultaneous elimination of the components characterised by a specific catalyst
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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
- B01J23/48—Silver or gold
- B01J23/52—Gold
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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
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
A kind of (Au, Rh)-Ce applied to NO+CO reactionx/Al2O3Preparation method, belong to catalysis material and technical field of nanometer material preparation.Use NaBH4Gold is supported on carrier with rhodium as reducing agent and using deposition-precipitation method, is dispersed in nano metal on carrier to get Aux‑Rh1‑x/Al2O3Catalyst.In order to improve the catalytic activity of catalyst, Ce is introduced using infusion process, obtains (Au, Rh)-Cex/Al2O3Catalyst.This preparation method is simple, and reaction condition is easily controllable, low for equipment requirements, (Au, Rh)-Ce obtainedx/Al2O3Material gold particle surface area is in 160m2/ g or so.Test condition: for 500ppm NO, 500ppm CO, He as balanced gas, the total flow of flue gas is 300ml/min, 250 DEG C at present denitration catalyst efficiency up to 100%.
Description
Technical field
The present invention is a kind of using NaBH4Reducing metal salt synthesizes alloy nanoparticle and passes through in water at room temperature
Infusion process synthesizes (Au, Rh)-Cex/Al2O3Method, belong to catalysis material and technical field of nanometer material preparation.The present invention answers
For prevention and control of air pollution field, it is related to (Au, Rh)-Cex/Al2O3Harmful NO and CO are converted to N for catalyst2With
CO2。
Background technique
Atmosphere pollution is increasingly serious, and atmosphere pollution state according to existing for it can be divided into particulate pollutant and gaseous contamination
Object, main pollutant have dust, sulfur dioxide (SO2), nitrogen oxides (NOx), carbon monoxide (CO), hydrocarbon etc..Greatly
Nitrogen oxides source in gas can be divided into natural pollution source and man-made pollution source, natural pollution source mainly have lightning stroke, volcano eruption,
Bacterial activity etc., artificial pollution mainly have thermal power plant, chemical plant, automobile and heating system etc..
Currently, there are mainly two types of the modes of elimination nitrogen oxides pollution, first is that improving combustion system inhibits NOxGeneration,
Second is that exhaust gas denitration.Although there are many method for removing nitrogen oxides, various methods have its corresponding defect and deficiency, from
And their extensive use is limited, and in comparison catalytic eliminating method has lower cost of investment, higher removing effect
Rate, therefore be a kind of more promising method.Catalyst used in catalytic eliminating method mainly has noble metal catalyst
With non-precious metal catalyst.
Noble metal catalyst is in selective catalytic reduction using earliest catalyst, the catalytic activity of noble metal catalyst
Mainly influenced by the active component of noble metal and carrier.Although non-precious metal catalyst manufacturing cost is cheap, it
It can not all be mentioned in the same breath with noble metal catalyst in anti-poisoning capability, ignition and air-fuel ratio, therefore noble metal catalyst
Critically important status is still accounted in pot flue gas cleaning and purifying vehicle exhaust.Although one kind of gold and noble metal,
There is price advantage compared with the precious metal materials such as rhodium, palladium, also there are the reserves of relative abundance, the technology of Jin Huishou is also relatively pure
It is ripe.Therefore using gold come synthetic catalyst carry out catalysis reaction both can also obtain higher catalytic with relative reduction cost
Can, there is very extensive application prospect.
The catalytic activity of gold is influenced by carrier, therefore more effectively to play the catalytic activity of gold, needs to select
Suitable carrier, TiO2, CeO2, γ-Al2O3, ZnO etc. be all the common carrier of loaded catalyst, the present invention uses γ-
Al2O3As carrier, alumina support specific surface area with higher can make nano metal material effectively play its catalysis and live
Property.Rare earth metal Ce is the most abundant rare earth metal in the earth's crust.It not only has good storage oxygen and discharges the ability of oxygen, more may be used
It is acted synergistically with being played with noble metal, increases the catalytic activity and stability of noble metal catalyst, CeO2It can be more as carrier
Disperse noble metal in Oxide-supports, to increase the activity and stability of catalyst.Some researches show that Ce not only
It can change the activation energy of CO oxidation reaction, oxygen vacancies can also be provided on the surface of catalyst after being reduced, so that NO is more
It is easy to dissociate, and conversion of the cerium between trivalent and tetravalence can significantly influence the reduction of NO.Research in recent years is aobvious
Show, the interaction due to transfer of the electronics between gold and metal oxide, between golden partial size and gold and support oxide
It is most important to catalytic performance.
Summary of the invention
For existing catalyst in reaction temperature height, anti-poisoning capability, the deficiency etc. on ignition and air-fuel ratio is asked
Topic, the present invention use NaBH first4Reducing metal salt synthesizes Au in water at room temperaturex-Rh1-x/Al2O3Catalyst, then lead to
It crosses infusion process and introduces transition metal Ce, final synthesis can efficiently remove catalyst (Au, Rh)-Ce of NO and CO at low temperaturex/
Al2O3。
Technical solution of the present invention:
A kind of (Au, Rh)-Ce applied to NO+CO reactionx/Al2O3Preparation method, steps are as follows:
1)Au-Rh/Al2O3Preparation: by HAuCl4With RhCl3·3H21:1 is mixedly configured into mixed solution to O in molar ratio,
Wherein, HAuCl4Concentration be 1.7mg/L；PEG-2000 is added into mixed solution, stirs 5-30min；Add Al2O3It carries
Body continues to stir 30min；Under constant agitation, NaBH is slowly added dropwise4Solution, then persistently stir 1h；Then to above-mentioned mixed
Solution after conjunction carries out dehydrated alcohol washing and centrifugation, repeats 3-5 times；By the sample drying after centrifuge washing, Au-Rh/ is obtained
Al2O3Powder；
Wherein, the gross mass and Al of gold and rhodium2O3Mass ratio be 3:100；
PEG-2000、NaBH4With Al2O3Mass ratio be 1:2.5:5；
2)(Au,Rh)-Cex/Al2O3Preparation: the Au-Rh/Al that step 1) is obtained2O3Powder is dissolved in deionized water,
Cerous nitrate is added after stirring sufficiently, makes Au-Rh/Al2O3The ratio between amount of substance of (Au, Rh) and Ce is 1:0.5-5 in powder, after
Continuous stirring 1h；Suspension is transferred in the round-bottomed flask of Rotary Evaporators after mixing and immerses temperature and maintains 60 DEG C
In water-bath, this keeps rotation 1h under atmospheric pressure；Then 35 DEG C are cooled to, vacuumize at this time and continues that rotation is kept to make to suspend
Solvent evaporation in liquid；Finally obtained solid sample is placed in air dry oven and is dried overnight, (Au, Rh)-is obtained
Cex/Al2O3。
(Au, Rh)-Ce of above-mentioned preparationx/Al2O3Catalyst is for handling the flue gas containing NO and CO, the test condition of reaction
Are as follows: 500ppm NO, 500ppm CO, He is as balanced gas.The total flow of flue gas is 300ml/min, the volume of catalyst
Air speed is 30,000ml/g-catalyst/h, and active testing temperature is 50-400 DEG C.
Beneficial effects of the present invention: the method that the present invention proposes synthesis nanometer bi-metal catalyst, obtained sample compare table
Area is about 160m2/g.The synthesis of nanometer bi-metal catalyst of the present invention overcomes prior synthesizing method to need to carry out high-temperature calcination
The drawbacks of, simplified synthesis step is simultaneously energy saving, has important application value.Nanometer bi-metal catalyst has more
Aun+With Rh+Active site, catalytic activity is high, can reach higher removal efficiency in lower temperature, and can remove NO simultaneously
With two kinds of polluted gas of CO.
Detailed description of the invention
Fig. 1 is (Au, the Rh)-Ce preparedx/Al2O3X-ray diffractogram figure.
Fig. 2 (a) is (Au, the Rh)-Ce preparedx/Al2O3X-ray photoelectron spectroscopic analysis figure.
Fig. 2 (b) is (Au, the Rh)-Ce preparedx/Al2O3X-ray photoelectron spectroscopic analysis figure.
Fig. 2 (c) is (Au, the Rh)-Ce preparedx/Al2O3X-ray photoelectron spectroscopic analysis figure.
Fig. 3 (a) is (Au, the Rh)-Ce preparedx/Al2O3Reactivity test NO removal rate figure.
Fig. 3 (b) is (Au, the Rh)-Ce preparedx/Al2O3Reactivity test N2Selective figure.
Specific embodiment
A specific embodiment of the invention is described in detail below in conjunction with technical solution.
Embodiment 1:Au-Rh/Al2O3Preparation method.
By HAuCl4With RhCl3·3H2O is that 1:1 is mixedly configured into 50mL solution by the mass ratio of the material of Au and Rh element,
Wherein HAuCl4Concentration be 1.7mg/L.The PEG-2000 of 0.16g is added into solution, stirs 5-30min.2.5g is added
Al2O3Carrier continues to stir 30min, 100 μ L 20mg mL is then slowly added dropwise into solution in whipping process-1NaBN4
Solution, then persistently stir 1h.After the completion of stirring, dehydrated alcohol washing and centrifugation are carried out to solution, repeated 3-5 times.Centrifugation is washed
Sample after washing is placed in 48h in 60 DEG C of air dry ovens and dries.
Embodiment 2:(Au, Rh)-Cex/Al2O3Preparation method.
The Au-Rh/Al for taking 4 parts of 1.5g above-mentioned2O3Powder is dissolved in being added after stirring sufficiently in 50mL deionized water
The cerous nitrate of 0.082g, 0.165g, 0.329g, 0.823g are pressed, and 1h is stirred.Suspension is transferred to rotary evaporation after mixing
It in the round-bottomed flask of instrument and immerses temperature and maintains in 60 DEG C of water-bath, this keeps rotating 1h under atmospheric pressure；Then cool down
To 35 DEG C, vacuumizes at this time and continue that rotation is kept to evaporate the solvent in suspension.Finally obtained solid sample is set
It is dried overnight in 60 DEG C of drying box, obtains (Au, Rh)-Cex/Al2O3。
Embodiment 3:(Au, Rh)-Cex/Al2O3The activation of catalyst.
By (Au, Rh)-Cex/Al2O3Catalyst is fitted into reactor.Use the pure H of 100mL/min flow velocity2, with 5 DEG C/
The heating rate of min is handled 1 hour at 300 DEG C.
Embodiment 4:(Au, Rh)-Cex/Al2O3The out of stock active testing of catalyst.
It is 8.2mm that catalyst sample after taking the above-mentioned activation of 0.3g, which is packed into internal diameter, and catalyst bed lengths are the stainless of 550mm
In steel pipe reactor.Reaction condition are as follows: 500ppm NO, 500ppm CO, He is as balanced gas.Above-mentioned gas mixing is passed through dress
Have in the reactor of catalyst, and by nitrogen-oxide analyzer, and gas chromatograph record NO concentration at different temperatures with
N2Concentration values.When temperature reaches 250 DEG C, denitration activity is up to 100%.
Embodiment 5:(Au, Rh)-Cex/Al2O3The characterization of catalyst.
BET: the catalyst sample after taking above-mentioned activation carries out compressing tablet process (pressure is about 6MPa), by sample at 150 DEG C
Lower degassing 1h is to remove the absorption water on catalyst surface and hole.Catalyst specific surface is measured using specific surface area analysis instrument
Product, pore volume and aperture.(Au,Rh)-Cex/Al2O3The specific surface area of catalyst is in 160m2/ g or so.
XRD: the catalyst sample after taking above-mentioned activation carries out compressing tablet process (pressure is about 6MPa), in X-ray diffractometer
It is upper that X-ray diffraction (XRD) measurement is carried out at 60kV and 55mA using CuK α radiation.It can clearly be observed that by adding Ce
Au (111), Au (200), the peak of Au (220) and Au (311) show that the presence of Ce may promote Au in bimetallic catalyst by oxygen
Compound state is transferred to reduction-state, to promote the electronics transfer from Au to Rh.
XPS: the catalyst sample after taking above-mentioned activation carries out compressing tablet process (pressure is about 6MPa), by using XPS light
The surface composition and oxidation state of electron spectrometer inspection catalyst surface.Ce3+Concentration with (Au, Rh)-Cex/Al2O3In
The increase of the amount of Ce and reduce, and (Au, Rh)-Ce (1:1)/Al2O3Middle Ce3+Concentration be higher than Ce/Al2O3.Au 4f and Rh
3d shows the positive displacement of respectively 40.0eV and 307.7eV.Above-mentioned behavior shows that there may be the electronics from metal to Ce
Transfer, the high catalytic activity for making it have high oxygen storage capacity and being dissociated for NO.
Table 1 (Au, Rh)-Cex/Al2O3Specific surface area and X-ray photoelectron spectroscopic analysis table.
Claims (2)
1. a kind of (Au, Rh)-Ce applied to NO+CO reactionx/Al2O3Preparation method, which is characterized in that steps are as follows:
1)Au-Rh/Al2O3Preparation: by HAuCl4With RhCl3·3H21:1 is mixedly configured into mixed solution to O in molar ratio,
In, HAuCl4Concentration be 1.7mg/L；PEG-2000 is added into mixed solution, stirs 5-30min；Add Al2O3Carrier,
Continue to stir 30min；Under constant agitation, NaBH is slowly added dropwise4Solution, then persistently stir 1h；Then to above-mentioned mixing
Solution afterwards carries out dehydrated alcohol washing and centrifugation, repeats 3-5 times；By the sample drying after centrifuge washing, Au-Rh/ is obtained
Al2O3Powder；
Wherein, the gross mass and Al of gold and rhodium2O3Mass ratio be 3:100；
PEG-2000、NaBH4With Al2O3Mass ratio be 1:2.5:5；
2)(Au,Rh)-Cex/Al2O3Preparation: the Au-Rh/Al that step 1) is obtained2O3Powder is dissolved in deionized water, stirring
Cerous nitrate is added after sufficiently, makes Au-Rh/Al2O3The ratio between amount of substance of (Au, Rh) and Ce is 1:0.5-5 in powder, continues to stir
Mix 1h；Suspension is transferred in the round-bottomed flask of Rotary Evaporators to after mixing and is immersed the water-bath that temperature is 60 DEG C
In, rotation 1h is kept under atmospheric pressure；Then 35 DEG C are cooled to, vacuumize and continues that rotation is kept to steam the solvent in suspension
Hair；It is finally that obtained solid sample is dry, obtain (Au, Rh)-Cex/Al2O3。
2. (Au, Rh)-Ce that preparation method described in claim 1 obtainsx/Al2O3Application, which is characterized in that will (Au,
Rh)-Cex/Al2O3Catalyst is for handling the flue gas containing NO and CO, the test condition of reaction are as follows: 500ppm NO, 500ppm
CO, He are as balanced gas；The total flow of flue gas is 300ml/min, and the air speed of the volume of catalyst is 30,000ml/g- catalysis
Agent/h, active testing temperature are 50-400 DEG C.
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| CN112892547B (en) * | 2021-01-18 | 2022-12-02 | 北京科技大学 | Catalyst for simultaneously removing nitrogen oxide and carbon monoxide and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101380575A (en) * | 2008-10-28 | 2009-03-11 | 华东理工大学 | High stability nano gold catalyst for CO normal temperature oxidation and preparation method thereof |
| CN103370153A (en) * | 2011-03-04 | 2013-10-23 | 丰田自动车株式会社 | Metal particles, catalyst for exhaust gas purification containing same, and production method therefor |
| CN105833867A (en) * | 2016-04-22 | 2016-08-10 | 大连理工大学 | Preparation method for Au-Ce/AlTiOx applied to NO+CO reaction and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101380575A (en) * | 2008-10-28 | 2009-03-11 | 华东理工大学 | High stability nano gold catalyst for CO normal temperature oxidation and preparation method thereof |
| CN103370153A (en) * | 2011-03-04 | 2013-10-23 | 丰田自动车株式会社 | Metal particles, catalyst for exhaust gas purification containing same, and production method therefor |
| CN105833867A (en) * | 2016-04-22 | 2016-08-10 | 大连理工大学 | Preparation method for Au-Ce/AlTiOx applied to NO+CO reaction and application thereof |
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