CN106582638A - Preparation method of (Au,Rh)-Cex/Al2O3 applied to NO+CO reaction - Google Patents
Preparation method of (Au,Rh)-Cex/Al2O3 applied to NO+CO reaction Download PDFInfo
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- CN106582638A CN106582638A CN201611226042.2A CN201611226042A CN106582638A CN 106582638 A CN106582638 A CN 106582638A CN 201611226042 A CN201611226042 A CN 201611226042A CN 106582638 A CN106582638 A CN 106582638A
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- 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
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- B01D53/8643—Removing mixtures of carbon monoxide or hydrocarbons and nitrogen oxides
- B01D53/8646—Simultaneous elimination of the components
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Abstract
The invention provides a preparation method of (Au,Rh)-Cex/Al2O3 applied to a NO+CO reaction, and belongs to the technical field of catalyst material and nanomaterial preparation. Gold and rhodium are loaded to a carrier by using NaBH4 as a reducing agent through a deposition precipitation method, the nanometals are dispersed on the carrier, and then a Aux-Rh1-x/Al2O3 catalyst is obtained. For improving the catalytic activity of the catalyst, Ce is introduced through a dipping method, and the (Au,Rh)-Cex/Al2O3 catalyst is obtained. The preparation method is simple, the reaction conditions are easy to control, the requirement on equipment is low, and the gold particle surface area of the prepared (Au,Rh)-Cex/Al2O3 material is about 160 m<2>/g. Testing is conducted under the conditions that 500 ppm NO, 500 PPM CO and He serve as equilibrium gases, the total flow of flue gas is 300 ml/min, and the denitration catalysis efficiency reaches 100% at 250 DEG C.
Description
Technical field
The present invention is that one kind uses NaBH4At room temperature in water reducing metal salt synthesizing alloy nanoparticle and pass through
Infusion process synthesizes (Au, Rh)-Cex/Al2O3Method, belong to catalysis material and technical field of nanometer material preparation.The present invention should
For prevention and control of air pollution field, it is related to (Au, Rh)-Cex/Al2O3Harmful NO and CO are changed into into N for catalyst2With
CO2。
Background technology
Atmospheric pollution is day by day serious, and atmosphere pollution can be divided into particulate pollutant and gaseous contamination according to its state for existing
Thing, 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 thunderbolt, volcano eruption,
The aspects such as bacterial activity, artificial pollution mainly have thermal power plant, chemical plant, automobile and heating system etc..
At present, the mode for eliminating nitrogen oxides pollution mainly has two kinds, and one is to improve combustion system to suppress NOxGeneration,
Two is exhaust gas denitration.Although the method for removing nitrogen oxides is a lot, various methods have its corresponding defect and deficiency, from
And their extensive application is limited, and catalytic eliminating method is comparatively speaking with relatively low cost of investment, higher removing effect
Rate, therefore be a kind of rising method of comparison.The catalyst used by catalytic eliminating method mainly has noble metal catalyst
With non-precious metal catalyst.
Noble metal catalyst is catalyst earliest used in SCR, the catalysis activity of noble metal catalyst
Mainly affected by the active component and kind of carrier of noble metal.Non-precious metal catalyst is although cheap for manufacturing cost, but it
All cannot mention in the same breath with noble metal catalyst in anti-poisoning capability, ignition and air-fuel ratio, therefore noble metal catalyst
Still critically important status is accounted in pot flue gas cleaning and purifying vehicle exhaust.Although one kind of gold and noble metal,
With price advantage compared with the precious metal materials such as rhodium, palladium, also there are the reserves of relative abundance, the technology that gold is reclaimed is also relatively pure
It is ripe.Therefore take synthetic catalyst using gold and carry out catalytic reaction both can to obtain higher catalytic with relative reduction cost
Can, with application prospect widely.
The catalysis activity of gold is affected by kind of carrier, therefore the catalysis activity more effectively to play gold, needs to select
Suitable carrier, TiO2, CeO2, γ-Al2O3, ZnO etc. be all the conventional carrier of loaded catalyst, the present invention using γ-
Al2O3Used as carrier, alumina support has higher specific surface area, nano metal material can be made effectively to play its catalysis and lived
Property.Rare earth metal Ce is most abundant rare earth metal in the earth's crust.It does not only have good storage oxygen and the ability of release oxygen, more may be used
Synergism is played with noble metal, increase the catalysis activity and stability of noble metal catalyst, CeO2Can be more as carrier
Noble metal is made well to disperse in Oxide-supports, so as to increase the activity and stability of catalyst.There are some researches show Ce not only
The activation energy of CO oxidation reactions can be changed, can be with the surface offer oxygen vacancies after being reduced in catalyst so that NO is more
It is easy to dissociation, and conversion of the cerium between trivalent and tetravalence can significantly affects the reduction of NO.Research in recent years shows
Show, due to transfer of the electronics between gold and metal-oxide, the particle diameter of gold and the interaction between gold and support oxide
It is most important to catalytic performance.
The content of the invention
For existing catalyst, in reaction temperature, high, anti-poisoning capability, the deficiency on ignition and air-fuel ratio etc. are asked
Topic, the present invention is first by NaBH4At room temperature in water reducing metal salt synthesizing Aux-Rh1-x/Al2O3Catalyst, then lead to
Cross infusion process and introduce transition metal Ce, final synthesis can efficiently remove catalyst (Au, the Rh)-Ce of NO and CO at low temperaturex/
Al2O3。
Technical scheme：
A kind of (Au, Rh)-Ce for being applied to NO+CO reactionsx/Al2O3Preparation method, step is as follows：
1)Au-Rh/Al2O3Preparation：By HAuCl4With RhCl3·3H2O in molar ratio 1:1 is mixedly configured into mixed solution,
Wherein, HAuCl4Concentration be 1.7mg/L；PEG-2000 is added in mixed solution, 5-30min is stirred；Add Al2O3Carry
Body, continues stirring 30min；Under constant agitation, it is slowly added dropwise NaBH4Solution, then persistently stir 1h；Then to above-mentioned mixed
Solution after conjunction carries out absolute ethanol washing and centrifugation, repeats 3-5 time；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：By step 1) Au-Rh/Al that obtains2O3Powder is dissolved in deionized water,
Cerous nitrate is added after stirring fully, Au-Rh/Al is made2O3In powder, (Au, Rh) and the ratio of the amount of the material of Ce are 1:0.5-5, after
Continuous stirring 1h；Suspension is transferred in the round-bottomed flask of Rotary Evaporators and immerses temperature after mix homogeneously and maintain 60 DEG C
In water-bath, this keeps rotating 1h under atmospheric pressure；Then 35 DEG C are cooled to, now evacuation and continue keep rotation make suspension
Solvent evaporation in liquid；Finally resulting solid sample is placed in air dry oven and is overnight dried, obtain (Au, Rh)-
Cex/Al2O3。
(Au, Rh)-Ce of above-mentioned preparationx/Al2O3Catalyst is used to process the flue gas containing NO and CO, the test condition of reaction
For：500ppm NO, 500ppm CO, He is used 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, the sample for obtaining 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, simplify synthesis step energy saving, with important using value.Nanometer bi-metal catalyst has more
Aun+With Rh+Avtive spot, catalysis activity are high, can reach higher removal efficiency in lower temperature, and can remove NO simultaneously
With two kinds of dusty gass of CO.
Description of the drawings
Fig. 1 is (Au, the Rh)-Ce for preparingx/Al2O3X-ray diffractogram figure.
Fig. 2 (a) is (Au, the Rh)-Ce for preparingx/Al2O3X-ray photoelectron spectroscopic analysis figure.
Fig. 2 (b) is (Au, the Rh)-Ce for preparingx/Al2O3X-ray photoelectron spectroscopic analysis figure.
Fig. 2 (c) is (Au, the Rh)-Ce for preparingx/Al2O3X-ray photoelectron spectroscopic analysis figure.
Fig. 3 (a) is (Au, the Rh)-Ce for preparingx/Al2O3Reactivity test NO clearance figures.
Fig. 3 (b) is (Au, the Rh)-Ce for preparingx/Al2O3Reactivity test N2Selective figure.
Specific embodiment
The specific embodiment of the present invention is described in detail below in conjunction with technical scheme.
Embodiment 1：Au-Rh/Al2O3Preparation method.
By HAuCl4With RhCl3·3H2It is 1 that O presses the amount ratio of the material of Au and Rh elements:1 is mixedly configured into 50mL solution,
Wherein HAuCl4Concentration be 1.7mg/L.The PEG-2000 of 0.16g is added in solution, 5-30min is stirred.Add 2.5g
Al2O3Carrier, continues stirring 30min, is then slowly added dropwise 100 μ L 20mg mL in whipping process in solution-1NaBN4
Solution, then persistently stir 1h.After the completion of stirring, absolute ethanol washing and centrifugation are carried out to solution, is repeated 3-5 time.Centrifugation is washed
Sample after washing is positioned over 48h drying in 60 DEG C of air dry ovens.
Embodiment 2：(Au,Rh)-Cex/Al2O3Preparation method.
Take 4 parts of above-mentioned Au-Rh/Al of 1.5g2O3During powder is dissolved in 50mL deionized waters, stirring fully rear addition is respectively
The cerous nitrate of 0.082g, 0.165g, 0.329g, 0.823g is pressed, and stirs 1h.Suspension is transferred to into rotary evaporation after mix homogeneously
The round-bottomed flask of instrument is interior and immerses in the water-bath that temperature maintains 60 DEG C, and this keeps rotating 1h under atmospheric pressure；Then lower the temperature
To 35 DEG C, now evacuation continue to keep rotation to make the evaporation of the solvent in suspension.Finally resulting solid sample is put
Overnight dry in 60 DEG C of drying baker, obtain (Au, Rh)-Cex/Al2O3。
Embodiment 3：(Au,Rh)-Cex/Al2O3The activation of catalyst.
By (Au, Rh)-Cex/Al2O3Catalyst loads in reactor.Using the pure H of 100mL/min flow velocitys2, with 5 DEG C/
The heating rate of min is processed 1 hour at 300 DEG C.
Embodiment 4：(Au,Rh)-Cex/Al2O3The out of stock active testing of catalyst.
Take the catalyst sample after the above-mentioned activation of 0.3g to load internal diameter is 8.2mm, and catalyst bed lengths are the stainless of 550mm
In steel pipe reactor.Reaction condition is：500ppm NO, 500ppm CO, He is used as balanced gas.Above-mentioned gas mixing is passed through dress
In having 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 sign of catalyst.
BET：Taking the catalyst sample after above-mentioned activation carries out compressing tablet process (pressure is about 6MPa), by sample at 150 DEG C
Lower degassing 1h with remove on catalyst surface and hole in absorption water.Catalyst specific surface is determined 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:Taking the catalyst sample after above-mentioned activation carries out compressing tablet process (pressure is about 6MPa), in X-ray diffractometer
Upper use CuK α radiation carries out X-ray diffraction (XRD) measurement under 60kV and 55mA.Can clearly be observed that by adding Ce
The peak of Au (111), Au (200), Au (220) and Au (311), shows that the presence of Ce may promote Au in bimetallic catalyst by oxygen
Compound state is transferred to reduction-state, so as to promote the electron transfer from Au to Rh.
XPS:Taking the catalyst sample after above-mentioned activation carries out compressing tablet process (pressure is about 6MPa), by using XPS light
Electron spectrometer checks the surface composition and oxidation state of 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 to there may be the electronics from metal to Ce
Transfer so as to high oxygen storage capacity and the high catalytic activity for NO dissociations.
Table 1 (Au, Rh)-Cex/Al2O3Specific surface area and X-ray photoelectron spectroscopic analysis table.
Claims (2)
1. it is a kind of to be applied to (Au, Rh)-Ce that NO+CO reactsx/Al2O3Preparation method, it is characterised in that step is as follows：
1)Au-Rh/Al2O3Preparation：By HAuCl4With RhCl3·3H2O in molar ratio 1:1 is mixedly configured into mixed solution, its
In, HAuCl4Concentration be 1.7mg/L；PEG-2000 is added in mixed solution, 5-30min is stirred；Add Al2O3Carrier,
Continue stirring 30min；Under constant agitation, it is slowly added dropwise NaBH4Solution, then persistently stir 1h；Then to above-mentioned mixing
Solution afterwards carries out absolute ethanol washing and centrifugation, repeats 3-5 time；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：By step 1) Au-Rh/Al that obtains2O3Powder is dissolved in deionized water, stirring
Cerous nitrate is added after fully, Au-Rh/Al is made2O3In powder, (Au, Rh) and the ratio of the amount of the material of Ce are 1:0.5-5, continues to stir
Mix 1h；Suspension is transferred in the round-bottomed flask of Rotary Evaporators after mix homogeneously and immerses the water-bath that temperature is 60 DEG C
In, rotation 1h is kept under atmospheric pressure；Then 35 DEG C are cooled to, evacuation simultaneously continues the solvent steaming during holding rotation makes suspension
Send out；Finally resulting solid sample is dried, (Au, Rh)-Ce is obtainedx/Al2O3。
2. (Au, Rh)-Ce that the preparation method described in claim 1 is obtainedx/Al2O3Application, it is characterised in that will (Au,
Rh)-Cex/Al2O3Catalyst is used to process the flue gas containing NO and CO, and the test condition of reaction is：500ppm NO, 500ppm
CO, He are used 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-
Catalyst/h, active testing temperature are 50-400 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111266123A (en) * | 2019-12-31 | 2020-06-12 | 南京环福新材料科技有限公司 | Multifunctional catalyst for purification and preparation method and application thereof |
| CN112892547A (en) * | 2021-01-18 | 2021-06-04 | 北京科技大学 | Catalyst for simultaneously removing nitrogen oxide and carbon monoxide and preparation method thereof |
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|---|---|---|---|---|
| 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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Patent 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111266123A (en) * | 2019-12-31 | 2020-06-12 | 南京环福新材料科技有限公司 | Multifunctional catalyst for purification and preparation method and application thereof |
| CN111266123B (en) * | 2019-12-31 | 2023-03-10 | 南京环福新材料科技有限公司 | Multifunctional catalyst for purification and preparation method and application thereof |
| CN112892547A (en) * | 2021-01-18 | 2021-06-04 | 北京科技大学 | Catalyst for simultaneously removing nitrogen oxide and carbon monoxide and preparation method thereof |
| 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 |
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